Search results for: emulsion solvent evaporation

Authors: Ahmad Kayvani Fard, Yehia Manawi

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Qatar’s primary source of fresh water is through seawater desalination. Amongst the major processes that are commercially available on the market, the most common large scale techniques are Multi-Stage Flash distillation (MSF), Multi Effect distillation (MED), and Reverse Osmosis (RO). Although commonly used, these three processes are highly expensive down to high energy input requirements and high operating costs allied with maintenance and stress induced on the systems in harsh alkaline media. Beside that cost, environmental footprint of these desalination techniques are significant; from damaging marine eco-system, to huge land use, to discharge of tons of GHG and huge carbon footprint. Other less energy consuming techniques based on membrane separation are being sought to reduce both the carbon footprint and operating costs is membrane distillation (MD). Emerged in 1960s, MD is an alternative technology for water desalination attracting more attention since 1980s. MD process involves the evaporation of a hot feed, typically below boiling point of brine at standard conditions, by creating a water vapor pressure difference across the porous, hydrophobic membrane. Main advantages of MD compared to other commercially available technologies (MSF and MED) and specially RO are reduction of membrane and module stress due to absence of trans-membrane pressure, less impact of contaminant fouling on distillate due to transfer of only water vapor, utilization of low grade or waste heat from oil and gas industries to heat up the feed up to required temperature difference across the membrane, superior water quality, and relatively lower capital and operating cost. To achieve the objective of this study, state of the art flat-sheet cross-flow DCMD bench scale unit was designed, commissioned, and tested. The objective of this study is to analyze the characteristics and morphology of the membrane suitable for DCMD through SEM imaging and contact angle measurement and to study the water quality of distillate produced by DCMD bench scale unit. Comparison with available literature data is undertaken where appropriate and laboratory data is used to compare a DCMD distillate quality with that of other desalination techniques and standards. Membrane SEM analysis showed that the PTFE membrane used for the study has contact angle of 127º with highly porous surface supported with less porous and bigger pore size PP membrane. Study on the effect of feed solution (salinity) and temperature on water quality of distillate produced from ICP and IC analysis showed that with any salinity and different feed temperature (up to 70ºC) the electric conductivity of distillate is less than 5 μS/cm with 99.99% salt rejection and proved to be feasible and effective process capable of consistently producing high quality distillate from very high feed salinity solution (i.e. 100000 mg/L TDS) even with substantial quality difference compared to other desalination methods such as RO and MSF.

Keywords: membrane distillation, waste heat, seawater desalination, membrane, freshwater, direct contact membrane distillation

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Authors: Pesaru Vigneshwar Reddy, Parvathaneni Pavan

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Green organic chemistry which is the latest and one of the most researched topics now-a- days has been in demand since 1990’s. Majority of the research in green organic chemistry chemicals are some of the important starting materials for greater number of major chemical industries. The production of organic chemicals has raw materials (or) reagents for other application is major sector of manufacturing polymers, pharmaceuticals, pesticides, paints, artificial fibers, food additives etc. organic synthesis on a large scale compound to the labratory scale, involves the use of energy, basic chemical ingredients from the petro chemical sectors, catalyst and after the end of the reaction, seperation, purification, storage, packing distribution etc. During these processes there are many problems of health and safety for workers in addition to the environmental problems caused there by use and deposition as waste. Green chemistry with its 12 principles would like to see changes in conventional way that were used for decades to make synthetic organic chemical and the use of less toxic starting materials. Green chemistry would like to increase the efficiency of synthetic methods, to use less toxic solvents, reduce the stage of synthetic routes and minimize waste as far as practically possible. In this way, organic synthesis will be part of the effort for sustainable development Green chemistry is also interested for research and alternatives innovations on many practical aspects of organic synthesis in the university and research labaratory of institutions. By changing the methodologies of organic synthesis, health and safety will be advanced in the small scale laboratory level but also will be extended to the industrial large scale production a process through new techniques. The three key developments in green chemistry include the use of super critical carbondioxide as green solvent, aqueous hydrogen peroxide as an oxidising agent and use of hydrogen in asymmetric synthesis. It also focuses on replacing traditional methods of heating with that of modern methods of heating like microwaves traditions, so that carbon foot print should reduces as far as possible. Another beneficiary of this green chemistry is that it will reduce environmental pollution through the use of less toxic reagents, minimizing of waste and more bio-degradable biproducts. In this present paper some of the basic principles, approaches, and early achievements of green chemistry has a branch of chemistry that studies the laws of passing of chemical reactions is also considered, with the summarization of green chemistry principles. A discussion about E-factor, old and new synthesis of ibuprofen, microwave techniques, and some of the recent advancements also considered.

Keywords: energy, e-factor, carbon foot print, micro-wave, sono-chemistry, advancement

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Authors: Natalia Alzate-Carvajal, Diego A. Acevedo-Guzman, Victor Meza-Laguna, Mario H. Farias, Luis A. Perez-Rey, Edgar Abarca-Morales, Victor A. Garcia-Ramirez, Vladimir A. Basiuk, Elena V. Basiuk

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Direct covalent functionalization of prefabricated free-standing graphene oxide paper (GOP) is considered as the only approach suitable for systematic tuning of thermal, mechanical and electronic characteristics of this important class of carbon nanomaterials. At the same time, the traditional liquid-phase functionalization protocols can compromise physical integrity of the paper-like material up to its total disintegration. To avoid such undesirable effects, we explored the possibility of employing an alternative, solvent-free strategy for facile and nondestructive functionalization of GOP with two representative aliphatic amines, 1-octadecylamine (ODA) and 1,12-diaminododecane (DAD), as well as with two aromatic amines, 1-aminopyrene (AP) and 1,5-diaminonaphthalene (DAN). The functionalization was performed under moderate heating at 150-180 °C in vacuum. Under such conditions, it proceeds through both amidation and epoxy ring opening reactions. Comparative characterization of pristine and amine-functionalized GOP mats was carried out by using Fourier-transform infrared, Raman, and X-ray photoelectron spectroscopy (XPS), thermogravimetric (TGA) and differential thermal analysis, scanning electron and atomic force microscopy (SEM and AFM, respectively). Besides that, we compared the stability in water, wettability, electrical conductivity and elastic (Young's) modulus of GOP mats before and after amine functionalization. The highest content of organic species was obtained in the case of GOP-ODA, followed by GOP-DAD, GOP-AP and GOP-DAN samples. The covalent functionalization increased mechanical and thermal stability of GOP, as well as its electrical conductivity. The magnitude of each effect depends on the particular chemical structure of amine employed, which allows for tuning a given GOP property. Morphological characterization by using SEM showed that, compared to pristine graphene oxide paper, amine-modified GOP mats become relatively ordered layered assemblies, in which individual GO sheets are organized in a near-parallel pattern. Financial support from the National Autonomous University of Mexico (grants DGAPA-IN101118 and IN200516) and from the National Council of Science and Technology of Mexico (CONACYT, grant 250655) is greatly appreciated. The authors also thank David A. Domínguez (CNyN of UNAM) for XPS measurements and Dr. Edgar Alvarez-Zauco (Faculty of Science of UNAM) for the opportunity to use TGA equipment.

Keywords: amines, covalent functionalization, gas-phase, graphene oxide paper

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Authors: Eliane G. Tótoli, Hérida Regina N. Salgado

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Daptomycin is an important antimicrobial agent used in clinical practice nowadays, since it is very active against some Gram-positive bacteria that are particularly challenges for the medicine, such as methicillin-resistant Staphylococcus aureus (MRSA) and vancomycin-resistant Enterococci (VRE). The importance of environmental preservation has receiving special attention since last years. Considering the evident need to protect the natural environment and the introduction of strict quality requirements regarding analytical procedures used in pharmaceutical analysis, the industries must seek environmentally friendly alternatives in relation to the analytical methods and other processes that they follow in their routine. In view of these factors, green analytical chemistry is prevalent and encouraged nowadays. In this context, infrared spectroscopy stands out. This is a method that does not use organic solvents and, although it is formally accepted for the identification of individual compounds, also allows the quantitation of substances. Considering that there are few green analytical methods described in literature for the analysis of daptomycin, the aim of this work was the development and validation of a green analytical method for the quantification of this drug in lyophilized powder for injectable solution, by Fourier-transform infrared spectroscopy (FT-IR). Method: Translucent potassium bromide pellets containing predetermined amounts of the drug were prepared and subjected to spectrophotometric analysis in the mid-infrared region. After obtaining the infrared spectrum and with the assistance of the IR Solution software, quantitative analysis was carried out in the spectral region between 1575 and 1700 cm-1, related to a carbonyl band of the daptomycin molecule, and this band had its height analyzed in terms of absorbance. The method was validated according to ICH guidelines regarding linearity, precision (repeatability and intermediate precision), accuracy and robustness. Results and discussion: The method showed to be linear (r = 0.9999), precise (RSD% < 2.0), accurate and robust, over a concentration range from 0.2 to 0.6 mg/pellet. In addition, this technique does not use organic solvents, which is one great advantage over the most common analytical methods. This fact contributes to minimize the generation of organic solvent waste by the industry and thereby reduces the impact of its activities on the environment. Conclusion: The validated method proved to be adequate to quantify daptomycin in lyophilized powder for injectable solution and can be used for its routine analysis in quality control. In addition, the proposed method is environmentally friendly, which is in line with the global trend.

Keywords: daptomycin, Fourier-transform infrared spectroscopy, green analytical chemistry, quality control, spectrometry in IR region

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Authors: G. A. Oladosu1, P. O. Ogbodogbo, C. I. Makinde1, M. O. Tijani, O. A. Adegboyega

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Saprolegniasis is a major pathogenic infection that contributes significantly to poor hatching rates in incubated fish eggs in the Africa catfish hatchery in Nigeria. Malachite green known to be very effective against this condition has been banned because it is carcinogenic. There is, therefore, the need for other effective yet safer methods of controlling saprolegniasis in incubated fish eggs. A total of 50 ml crude, chloroform extract of pyocyanin from which solvent was removed to attain 30 ml, having a concentration of 12.16 ug/ml was produced from 700 ml broth culture of Pseudomonas aeruginosa isolated from a previous study. In-vitro susceptibility of the fungus was investigated by exposing fungal infected eggs to two different time-concentration ratios of pyocyanin; 0.275 ug/ml and 2.75 ug/ml for 1 and 24 hours, and 5 mg/L malachite green as positive control while normal saline was the control. The efficacy of pyocyanin was evaluated using the degree of mycelial growth inhibition in different treatments. Fertilized Clarias gariepinus eggs (between 45 to 64 eggs) were then incubated in 20 ml of medium containing similar concentrations of pyocyanin and malachite green, with freshwater as a control for 24 hours. Hatching rates of the incubated eggs were observed. Three samples of un-hatched eggs were taken from each medium and observed for the presence of fungal pathogens using microscopy. Another batch of three samples of un-hatched eggs from each treatment was also inoculated on Sabourand dextrose agar (SDA) using Egg-Agar Transfer Technique to observe for fungal growth. Mycelial growth was inhibited in fungal infected eggs treated with 2.75 ug/ml for 24 hrs and the 5 mg/L malachite green for both 1 hr and 24 hrs. The mortality rate was 100% in fertilized C. gariepinus eggs exposed for 24 hrs to 0.275 and 2.75 ug/ml of pyocyanin. The mortality rate was least in malachite green followed by the control treatment. Embryonic development was observed to be arrested in the eggs treated with the two pyocyanin concentrations as they maintain their colour but showed no development beyond the gastrula stage, whereas viable eggs in the control and malachite green treatments developed fully into healthy hatchlings. Furthermore, microscopy of the un-hatched eggs revealed the presence of a protozoan ciliate; Colpidium sp, (Tetrahymenidae), as well as a pathogenic fungus; Saprolegnia sp. in the control but not in the malachite green and pyocyanin treatments. Growth of Saprolegnia sp was also observed in SDA culture of un-hatched eggs from the control, but not from pyocyanin and malachite green treated eggs. Pyocyanin treatment of incubated eggs of Clarias gariepinus effectively prevented fungal infection in the eggs, but also arrested the development of the embryo. Therefore, crude chloroform extract of pyocyanin from Pseudomonas aeruginosa cannot be used in the control of Saprolegniasis in incubated Clarias gariepinus eggs at the concentration and duration tested in this study.

Keywords: African catfish, bioprophylaxis, catfish embryo, Saprolegniasis

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Authors: Michal Geca, Grzegorz Baranski, Ksenia Siadkowska

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The work is a part of the project which aims at developing innovative power and control systems for the high power aircraft piston engine ASz62IR. Developed electronically controlled ignition system will reduce emissions of toxic compounds as a result of lowered fuel consumption, optimized combustion and engine capability of efficient combustion of ecological fuels. The tested unit is an air-cooled four-stroke gasoline engine of 9 cylinders in a radial setup, mechanically charged by a radial compressor powered by the engine crankshaft. The total engine cubic capac-ity is 29.87 dm3, and the compression ratio is 6.4:1. The maximum take-off power is 1000 HP at 2200 rpm. The maximum fuel consumption is 280 kg/h. Engine powers aircrafts: An-2, M-18 „Dromader”, DHC-3 „OTTER”, DC-3 „Dakota”, GAF-125 „HAWK” i Y5. The main problems of the engine includes the imbalanced work of cylinders. The non-uniformity value in each cylinder results in non-uniformity of their work. In radial engine cylinders arrangement causes that the mixture movement that takes place in accordance (lower cylinder) or the opposite (upper cylinders) to the direction of gravity. Preliminary tests confirmed the presence of uneven workflow of individual cylinders. The phenomenon is most intense at low speed. The non-uniformity is visible on the waveform of cylinder pressure. Therefore two studies were conducted to determine the impact of this phenomenon on the engine performance: simulation and real tests. Simplified simulation was conducted on the element of the intake system coated with fuel film. The study shows that there is an effect of gravity on the movement of the fuel film inside the radial engine intake channels. Both in the lower and the upper inlet channels the film flows downwards. It follows from the fact that gravity assists the movement of the film in the lower cylinder channels and prevents the movement in the upper cylinder channels. Real tests on aircraft engine ASz62IR was conducted in transients condition (rapid change of the excess air in each cylinder were performed. Calculations were conducted for mass of fuel reaching the cylinders theoretically and really and on this basis, the factors of fuel evaporation “x” were determined. Therefore a simplified model of the fuel supply to cylinder was adopted. Model includes time constant of the fuel film τ, the number of engine transport cycles of non-evaporating fuel along the intake pipe γ and time between next cycles Δt. The calculation results of identification of the model parameters are presented in the form of radar graphs. The figures shows the averages declines and increases of the injection time and the average values for both types of stroke. These studies shown, that the change of the position of the cylinder will cause changes in the formation of fuel-air mixture and thus changes in the combustion process. Based on the results of the work of simulation and experiments was possible to develop individual algorithms for ignition control. This work has been financed by the Polish National Centre for Research and Development, INNOLOT, under Grant Agreement No. INNOLOT/I/1/NCBR/2013.

Keywords: radial engine, ignition system, non-uniformity, combustion process

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Authors: Nidhi Sharotri, Dhiraj Sud

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Water pollution by pesticides constitutes a serious ecological problem due to their potential toxicity and bioaccumulation. The widespread use of pesticides in industry and agriculture along with their resistance to natural decomposition, biodegradation, chemical and photochemical degradation under typical environmental conditions has resulted in the emergence of these chemicals and their transformed products in natural water. Among AOP’s, heterogeneous photocatalysis using TiO2 as photocatalyst appears as the most emerging destructive technology for mineralization of the pollutant in aquatic streams. Among the various semiconductors (TiO2, ZnO, CdS, FeTiO3, MnTiO3, SrTiO2 and SnO2), TiO2 has proven to be the most efficient photocatalyst for environmental applications due to its biological and chemical inertness, high photo reactivity, non-toxicity, and photo stability. Semiconductor photocatalysts are characterized by an electronic band structure in which valence band and conduction band are separated by a band gap, i.e. a region of forbidden energy. Semiconductor based photocatalysts produces e-/h+ pairs which have been employed for degradation of organic pollutants. The present paper focuses on modification of TiO2 photocatalyst in order to shift its absorption edge towards longer wavelength to make it active under natural light. Semiconductor TiO2 photocatalysts was prepared by doping with anion (N), cation (Mn) and double doped (Mn, N) using greener approach. Titanium isopropoxide is used as titania precursor and ethanedithiol, hydroxyl amine hydrochloride, manganous chloride as sulphur, nitrogen and manganese precursors respectively. Synthesized doped TiO2 nanomaterials are characterized for surface morphology (SEM, TEM), crystallinity (XRD) and optical properties (absorption spectra and band gap). EPR data confirms the substitutional incorporation of Mn2+ in TiO2 lattice. The doping influences the phase transformation of rutile and anatase phase crystal and thereby the absorption spectrum changes were observed. The effect of variation of reaction parameters such as solvent, reaction time and calcination temperature on the yield, surface morphology and optical properties was also investigated. The TEM studies show the particle size of nanomaterials varies from 10-50 nm. The calculated band gap of nanomaterials varies from 2.30-2.60 eV. The photocatalytic degradation of organic pollutant organophosphate pesticide (Quinalphos) has been investigated by studying the changes in UV absorption spectrum and the promising results were obtained under visible light. The complete mineralization of quinalphos has occurred as no intermediates were recorded after 8 hrs of degradation confirmed from the HPLC studies.

Keywords: quinalphos, doped-TiO2, mineralization, EPR

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Authors: Belen Montero, Carmen Ramirez, Maite Rico, Rebeca Bouza, Irene Derungs

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Starch is a promising polymer for producing biocomposite materials because it is renewable, completely biodegradable and easily available at a low cost. Thermoplastic starches (TPS) can be obtained after the disruption and plasticization of native starch with a plasticizer. In this work, the solvent casting method was used to obtain TPS films from wheat starch plasticized with glycerol and reinforced with nanocellulose (CNC). X-ray diffraction analysis was used to follow the evolution of the crystallinity. The native wheat starch granules have shown a profile corresponding to A-type crystal structures typical for cereal starches. When TPS films are analyzed a high amorphous halo centered on 19º is obtained, indicating the plasticization process is completed. SEM imaging was made in order to analyse the morphology. The image from the raw wheat starch granules shows a bimodal granule size distribution with some granules in large round disk-shape forms (A-type) and the others as smaller spherical particles (B-type). The image from the neat TPS surface shows a continuous surface. No starch aggregates or swollen granules can be seen so, the plasticization process is complete. In the surfaces of reinforced TPS films aggregates are seen as the CNC concentration in the matrix increases. The CNC influence on the mechanical properties of TPS films has been studied by dynamic mechanical analysis. A direct relation exists between the storage modulus values, E’, and the CNC content in reinforced TPS films: higher is the content of nanocellulose in the composite, higher is the value of E’. This reinforcement effect can be explained by the appearance of a strong and crystalline nanoparticle-TPS interphase. Thermal stability of films was analysed by TGA. It has not observed any influence on the behaviour related to the thermal degradation of films with the incorporation of the CNC. Finally, the resistance to the water absorption films was analysed following the standard UNE-EN ISO 1998:483. The percentage of water absorbed by the samples at each time was calculated. The addition of 5 wt % of CNC to the TPS matrix leads to a significant improvement in the moisture resistance of the starch based material decreasing their diffusivity. It has been associated to the formation of a nanocrystal network that prevents swelling of the starch and therefore water absorption and to the high crystallinity of cellulose compared to starch. As a conclusion, the wheat film reinforced with 5 wt % of cellulose nanocrystals seems to be a good alternative for short-life applications into the packaging industry, because of its greatest rigidity, thermal stability and moisture sorption resistance.

Keywords: biocomposites, nanocellulose, starch, wheat

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Authors: I. Berger, N. Machour, F. Portet-Koltalo

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Polycyclic aromatic hydrocarbons (PAHs) are toxic and carcinogenic pollutants produced in majority by incomplete combustion processes in industrialized and urbanized areas. After being emitted in atmosphere, these persistent contaminants are deposited to soils or sediments. Even if persistent, some can be partially degraded (photodegradation, biodegradation, chemical oxidation) and they lead to oxygenated metabolites (oxy-PAHs) which can be more toxic than their parent PAH. Oxy-PAHs are less measured than PAHs in sediments and this study aims to compare different analytical tools in order to extract and quantify a mixture of four hydroxylated PAHs (OH-PAHs) and four carbonyl PAHs (quinones) in sediments. Methodologies: Two analytical systems – HPLC with on-line UV and fluorescence detectors (HPLC-UV-FLD) and GC coupled to a mass spectrometer (GC-MS) – were compared to separate and quantify oxy-PAHs. Microwave assisted extraction (MAE) was optimized to extract oxy-PAHs from sediments. Results: First OH-PAHs and quinones were analyzed in HPLC with on-line UV and fluorimetric detectors. OH-PAHs were detected with the sensitive FLD, but the non-fluorescent quinones were detected with UV. The limits of detection (LOD)s obtained were in the range (2-3)×10-4 mg/L for OH-PAHs and (2-3)×10-3 mg/L for quinones. Second, even if GC-MS is not well adapted to the analysis of the thermodegradable OH-PAHs and quinones without any derivatization step, it was used because of the advantages of the detector in terms of identification and of GC in terms of efficiency. Without derivatization, only two of the four quinones were detected in the range 1-10 mg/L (LODs=0.3-1.2 mg/L) and LODs were neither very satisfying for the four OH-PAHs (0.18-0.6 mg/L). So two derivatization processes were optimized, comparing to literature: one for silylation of OH-PAHs, one for acetylation of quinones. Silylation using BSTFA/TCMS 99/1 was enhanced using a mixture of catalyst solvents (pyridine/ethyle acetate) and finding the appropriate reaction duration (5-60 minutes). Acetylation was optimized at different steps of the process, including the initial volume of compounds to derivatize, the added amounts of Zn (0.1-0.25 g), the nature of the derivatization product (acetic anhydride, heptafluorobutyric acid…) and the liquid/liquid extraction at the end of the process. After derivatization, LODs were decreased by a factor 3 for OH-PAHs and by a factor 4 for quinones, all the quinones being now detected. Thereafter, quinones and OH-PAHs were extracted from spiked sediments using microwave assisted extraction (MAE) followed by GC-MS analysis. Several mixtures of solvents of different volumes (10-25 mL) and using different extraction temperatures (80-120°C) were tested to obtain the best recovery yields. Satisfactory recoveries could be obtained for quinones (70-96%) and for OH-PAHs (70-104%). Temperature was a critical factor which had to be controlled to avoid oxy-PAHs degradation during the MAE extraction process. Conclusion: Even if MAE-GC-MS was satisfactory to analyze these oxy-PAHs, MAE optimization has to be carried on to obtain a most appropriate extraction solvent mixture, allowing a direct injection in the HPLC-UV-FLD system, which is more sensitive than GC-MS and does not necessitate a previous long derivatization step.

Keywords: derivatizations for GC-MS, microwave assisted extraction, on-line HPLC-UV-FLD, oxygenated PAHs, polluted sediments

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Authors: Sakeena Naikwadi, K. Jagaluraiah Sannapapamma

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Vetiveria zizanioides is an aromatic grass and traditionally been used in aromatherapy and ayurvedic medicine. Vetiver root is multi-functional biopolymer and has highly aromatic, antimicrobial, UV blocking, antioxidant properties suitable for textile finishing. The vetiver root (Gulabi) powder of different concentration (2, 4, 6,8 percent) were extracted by aqueous and solvent methods subjected to bioassay for antimicrobial efficiency and GCMS spectral analysis. The organic cotton fabric was finished with vetiver root extract (8 percent) by exhaust and pad dry cure methods. The finished fabric was assessed for functional properties viz., UV protective factor, antimicrobial efficiency and aroma intensity. The results revealed that Ethanol extraction showed a greater zone of inhibition compared to aqueous extract in root powder. Among the concentrations, 8 percent root extract in ethanol showed a greater zone of inhibition against gram-positive organism S. aureus and gram-negative organism E. coli. The major compounds present in vetiver root extracts were diethyl pathalate with greater percentage (87.73 %) followed by 7- Isopropyl dimethyl carboxylic acid (4.05 %), 2-butanone 4-trimethyle cyclohexen (1.21 %), phenanthrene carboxylic acid (1.03 %), naphthalene pentanoic acid (0.99 %), 1-phenanthrene carboxylic acid and 1 cyclohexenone 2-methyl oxobuty (0.89 %). The sample finished by pad dry cure method exhibited better UV protection even after 10th wash as compared to exhaust method. Vetiver extract treated samples exhibited maximum zone of inhibition against S. aureus than the E. coli organism. The vetiver root extract treated organic cotton fabric through pad dry cure method possessed good antimicrobial activity against S. aureus and E. coli even after 20th washes compared to vetiver root extract treated by exhaust method. The olfactory analysis was carried out by 30 panels of members and opined that vetiver root extract treated fabric has very good and pleasant aroma with better tactile properties that provide cooling, soothing effect and enhances the mood of the wearer. Vetiver root extract finished organic cotton fabric possessed aroma, antimicrobial and UV properties which are aptly suitable for medical and healthcare textiles viz., wound dressing, bandage gauze, surgical cloths, baby diapers and sanitary napkins. It can be used as after finishing agent for variegated garments and made-ups and can be replaced with commercial after finishing agents.

Keywords: antimicrobial, olfactory analysis, UV protection factor, vetiver root extract

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Authors: Salvana P. M. Costa, Tarcyla A. Gomes, Giovanna C. R. M. Schver, Leslie R. M. Ferraz, Cristovão R. Silva, Magaly A. M. Lyra, Danilo A. F. Fonte, Larissa A. Rolim, Amanda C. Q. M. Vieira, Miracy M. Albuquerque, Pedro J. Rolim-neto

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Efavirenz (EFV) is considered one of the most widely used anti-HIV drugs. However, it is classified as a drug class II (poorly soluble, highly permeable) according to the biopharmaceutical classification system, presenting problems of absorption in the gastrointestinal tract and thereby inadequate bioavailability for its therapeutic action. This study aimed to overcome these barriers by developing and obtaining solid dispersions (SD) in order to increase the EFZ bioavailability. For the development of SD with EFV, theoretical and practical studies were initially performed. Thus, there was a choice of a carrier to be used. For this, it was analyzed the various criteria such as glass transition temperature of the polymer, intra- and intermolecular interactions of hydrogen bonds between drug and polymer, the miscibility between the polymer and EFV. The choice of the obtainment method of the SD came from the analysis of which method is the most consolidated in both industry and literature. Subsequently, the choice of drug and carrier concentrations in the dispersions was carried out. In order to obtain DS to present the drug in its amorphous form, as the DS were obtained, they were analyzed by X-ray diffraction (XRD). SD are more stable the higher the amount of polymer present in the formulation. With this assumption, a SD containing 10% of drug was initially prepared and then this proportion was increased until the XRD showed the presence of EFV in its crystalline form. From this point, it was not produced SD with a higher concentration of drug. Thus, it was allowed to select PVP-K30, PVPVA 64 and the SOLUPLUS formulation as carriers, once it was possible the formation of hydrogen bond between EFV and polymers since these have hydrogen acceptor groups capable of interacting with the donor group of the drug hydrogen. It is worth mentioning also that the films obtained, independent of concentration used, were presented homogeneous and transparent. Thus, it can be said that the EFV is miscible in the three polymers used in the study. The SD and Physical Mixtures (PM) with these polymers were prepared by the solvent method. The EFV diffraction profile showed main peaks at around 2θ of 6,24°, in addition to other minor peaks at 14,34°, 17,08°, 20,3°, 21,36° and 25,06°, evidencing its crystalline character. Furthermore, the polymers showed amorphous nature, as evidenced by the absence of peaks in their XRD patterns. The XRD patterns showed the PM overlapping profile of the drug with the polymer, indicating the presence of EFV in its crystalline form. Regardless the proportion of drug used in SD, all the samples showed the same characteristics with no diffraction peaks EFV, demonstrating the behavior amorphous products. Thus, the polymers enabled, effectively, the formation of amorphous SD, probably due to the potential hydrogen bonds between them and the drug. Moreover, the XRD analysis showed that the polymers were able to maintain its amorphous form in a concentration of up to 80% drug.

Keywords: amorphous form, Efavirenz, solid dispersions, solubility

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Authors: Velvizhi Dharmalingam, Rajalaksmi Ramalingam, Rekha Prabhu, Ilavarasan Raju

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Background: The use of herbal products for various therapeutic regimens has increased tremendously in the developing countries. Elaeocarpus ganitrus(Rudraksha) is a broad-leaved tree, belonging to the family Elaeocarpaceae found in tropical and subtropical areas. It is popular in an indigenous system of medicine like Ayurveda, Siddha, and Unani. According to Ayurvedic medicine, Rudraksha is used in the managing of blood pressure, asthma, mental disorders, diabetes, gynaecological disorders, neurological disorders such as epilepsy and liver diseases. Objectives: The present study aimed to study the physicochemical parameters of Elaeocarpus ganitrus(fruits) and identify the phenolic compounds (gallic acid, ellagic acid, and chebulinic acid). To estimate the microbial load and the antibacterial activity of extract of Elaeocarpus ganitrus for selective pathogens. Methodology: The dried powdered fruit of Elaeocarpus ganitrus was performed the physicochemical parameters (such as Loss on drying, Alcohol soluble extractive, Water soluble extractive, Total ash and Acid insoluble ash) and pH was measured. The dried coarse powdered fruit of Elaeocarpus ganitrus was extracted successively with hexane, chloroform, ethylacetate and aqueous alcohol by cold percolation method. Identification of phenolic compounds (gallic acid, ellagic acid, chebulinic acid) was done by HPTLC method and confirmed by co-TLC using different solvent system.The successive extracts of Elaeocarpus ganitrus and standards (like gallic acid, ellagic acid, and chebulinic acid) was approximately weighed and made up with alcohol. HPTLC (CAMAG) analysis was performed on a TLC over silica gel 60F254 precoated aluminium plate, layer thickness 0.2 mm (E.Merck, Germany) by using ATS4, Visualizer and Scanner with wavelength at 254 nm, 366 nm and derivatized with different reagents. The microbial load such as total bacterial count, total fungal count, Enterobacteria, Escherichia coli, Salmonella species, Staphylococcus aureus and Pseudomonas aeruginosa by serial dilution method and antibacterial activity of was measured by Kirby bauer method for selective pathogens. Results: The physicochemical parameter of Elaeocarpus ganitrus was studied for standardization of crude drug. Among all the successive extracts were identified with phenolic compounds and Elaeocarpus ganitrus extract having potent antibacterial activity against gram-positive and gram-negative bacteria.

Keywords: antimicrobial activity, Elaeocarpus ganitrus, HPTLC, phenolic compounds

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Authors: Majid Farsadrouh Rashti, Alireza Mohammadinejad, Amir Shafiee Kisomi

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Lead (Pb²⁺), a cation, is a prime constituent of the majority of the industrial effluents such as mining, smelting and coal combustion, Pb-based painting and Pb containing pipes in water supply systems, paper and pulp refineries, printing, paints and pigments, explosive manufacturing, storage batteries, alloy and steel industries. The maximum permissible limit of lead in the water used for drinking and domesticating purpose is 0.01 mg/L as advised by Bureau of Indian Standards, BIS. This becomes the acceptable 'safe' level of lead(II) ions in water beyond which, the water becomes unfit for human use and consumption, and is potential enough to lead health problems and epidemics leading to kidney failure, neuronal disorders, and reproductive infertility. Superabsorbent hydrogels are loosely crosslinked hydrophilic polymers that in contact with aqueous solution can easily water and swell to several times to their initial volume without dissolving in aqueous medium. Superabsorbents are kind of hydrogels capable to swell and absorb a large amount of water in their three-dimensional networks. While the shapes of hydrogels do not change extensively during swelling, because of tremendously swelling capacity of superabsorbent, their shape will broadly change.Because of their superb response to changing environmental conditions including temperature pH, and solvent composition, superabsorbents have been attracting in numerous industrial applications. For instance, water retention property and subsequently. Natural-based superabsorbent hydrogels have attracted much attention in medical pharmaceutical, baby diapers, agriculture, and horticulture because of their non-toxicity, biocompatibility, and biodegradability. Novel superabsorbent hydrogel nanocomposites were prepared by graft copolymerization of acrylamide and itaconic acid in the presence of nanoclay (laponite), using methylene bisacrylamide (MBA) and potassium persulfate, former as a crosslinking agent and the second as an initiator. The superabsorbent hydrogel nanocomposites structure was characterized by FTIR spectroscopy, SEM and TGA Spectroscopy adsorption of metal ions on poly (AAm-co-IA). The equilibrium swelling values of copolymer was determined by gravimetric method. During the adsorption of metal ions on polymer, residual metal ion concentration in the solution and the solution pH were measured. The effects of the clay content of the hydrogel on its metal ions uptake behavior were studied. The NC hydrogels may be considered as a good candidate for environmental applications to retain more water and to remove heavy metals.

Keywords: adsorption, hydrogel, nanocomposite, super adsorbent

Procedia PDF Downloads 165

Authors: Anitha Kandasamy, Thirumurugan Ramaiah

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Interestingly, organic materials exhibit large optical nonlinearity with quick responses and having the flexibility of molecular tailoring using computational modelling and favourable synthetic methodologies. Pyridine based organic compounds and carboxylic acid contained aromatic compounds play a crucial role in crystal engineering of NCS complexes that displays admirable optical nonlinearity with fast response and favourable physicochemical properties such as low dielectric constant, wide optical transparency and large laser damage threshold value requires for optoelectronics device applications. Based on these facts, it was projected to form an acentric molecule of π-conjugated system interaction with appropriately replaced electron donor and acceptor groups for achieving higher SHG activity in which quinoline-2-carboyxlic acid is chosen as an electron acceptor and capable of acting as an acid as well as a base molecule, while 2-amino-4-methylpyridine is used as an electron donor and previously employed in numerous proton transfer complexes for synthesis of NLO materials for optoelectronic applications. 2-amino-4-mehtylpyridinium quinoline-2-carboxylate molecular complex (2AQ) is having π-donor-acceptor groups in which 2-amino-4-methylpyridine donates one of its electron to quinoline -2-carboxylic acid thereby forming a protonated 2-amino-4-methyl pyridinium moiety and mono ionized quinoline-2-carboxylate moiety which are connected via N-H…O intermolecular interactions with non-centrosymmetric crystal packing arrangement at microscopic scale is accountable to the enhancement of macroscopic second order NLO activity. The 2AQ crystal was successfully grown by a slow evaporation solution growth technique and its structure was determined in orthorhombic crystal system with acentric, P212121, space group. Hirshfeld surface analysis reveals that O…H intermolecular interactions primarily contributed with 31.0 % to the structural stabilization of 2AQ. The molecular structure of title compound has been confirmed by 1H and 13C NMR spectral studies. The vibrational modes of functional groups present in 2AQ have been assigned by using FTIR and FT-Raman spectroscopy. The grown 2AQ crystal exhibits high optical transparency with lower cut-off wavelength (275 nm) within the region of 275-1500 nm. The laser study confirmed that 2AQ exhibits high SHG efficiency of 12.6 times greater than that of KDP. TGA-DTA analysis revealed that 2AQ crystal had a thermal stability of 223 °C. The low dielectric constant and low dielectric loss at higher frequencies confirmed good crystalline nature with fewer defects of grown 2AQ crystal. The grown crystal exhibits soft material and positive photoconduction behaviour. Mulliken atomic distribution and FMOs analysis suggested that the strong intermolecular hydrogen bonding which lead to the enhancement of NLO activity. These properties suggest that 2AQ crystal is a suitable material for optoelectronic and laser frequency conversion applications.

Keywords: crystal growth, NLO activity, proton transfer complex, quantum chemical investigation

Procedia PDF Downloads 101

Authors: Franciele L. Bernard, Felipe Dalla Vecchia, Barbara B. Polesso, Jose A. Donato, Marcus Seferin, Rosane Ligabue, Jailton F. do Nascimento, Sandra Einloft

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The increasing level of carbon dioxide concentration in the atmosphere related to fossil fuels processing and utilization are contributing to global warming phenomena considerably. Carbon capture and storage (CCS) technologies appear as one of the key technologies to reduce CO2 emissions mitigating the effects of climate change. Absorption using amines solutions as solvents have been extensively studied and used in industry for decades. However, solvent degradation and equipment corrosion are two of the main problems in this process. Poly (ionic liquid) (PIL) is considered as a promising material for CCS technology, potentially more environmentally friendly and lesser energy demanding than traditional material. PILs possess a unique combination of ionic liquids (ILs) features, such as affinity for CO2, thermal and chemical stability and adjustable properties, coupled with the intrinsic properties of the polymer. This study investigated new Poly (ionic liquid) (PIL) based on polyurethanes with different ionic liquids cations and its potential for CO2 capture. The PILs were synthesized by the addition of diisocyante to a difunctional polyol, followed by an exchange reaction with the ionic Liquids 1-butyl-3-methylimidazolium chloride (BMIM Cl); tetrabutylammonium bromide (TBAB) and tetrabutylphosphonium bromide (TBPB). These materials were characterized by Fourier transform infrared spectroscopy (FTIR), Proton Nuclear Magnetic Resonance (1H-NMR), Atomic force microscopy (AFM), Tensile strength analysis, Field emission scanning electron microscopy (FESEM), Thermogravimetric analysis (TGA), Differential scanning calorimetry (DSC). The PILs CO2 sorption capacity were gravimetrically assessed in a Magnetic Suspension Balance (MSB). It was found that the ionic liquids cation influences in the compounds properties as well as in the CO2 sorption. The best result for CO2 sorption (123 mgCO2/g at 30 bar) was obtained for the PIL (PUPT-TBA). The higher CO2 sorption in PUPT-TBA is probably linked to the fact that the tetraalkylammonium cation having a higher positive density charge can have a stronger interaction with CO2, while the imidazolium charge is delocalized. The comparative CO2 sorption values of the PUPT-TBA with different ionic liquids showed that this material has greater capacity for capturing CO2 when compared to the ILs even at higher temperature. This behavior highlights the importance of this study, as the poly (urethane) based PILs are cheap and versatile materials.

Keywords: capture, CO2, ionic liquids, ionic poly(urethane)

Procedia PDF Downloads 214

Authors: Auteleyeva Laura, Maikanov Balgabai, Smagulova Ayana

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In order to find and select detoxification methods, patent and information research was conducted, as a result of which 68 patents for inventions were found, among them from the near abroad - 14 (Russia), from far abroad: China – 27, USA - 6, South Korea–1, Germany - 2, Mexico – 4, Yugoslavia – 7, Austria, Taiwan, Belarus, Denmark, Italy, Japan, Canada for 1 security document. Aflatoxin B₁ in various nuts was determined by two methods: enzyme immunoassay "RIDASCREEN ® FAST Aflatoxin" with determination of optical density on a microplate spectrophotometer RIDA®ABSORPTION 96 with RIDASOFT® software Win.NET (Germany) and the method of high-performance liquid chromatography (HPLC Corporation Water, USA) according to GOST 307112001. For experimental contamination of nuts, the cultivation of strain A was carried out. flavus KWIK-STIK on the medium of Chapek (France) with subsequent infection of various nuts (peanuts, peanuts with shells, badam, walnuts with and without shells, pistachios).Based on our research, we have selected 2 detoxification methods: method 1 – combined (5% citric acid solution + microwave for 640 W for 3 min + UV for 20 min) and a chemical method with various leaves of plants: Artemisia terra-albae, Thymus vulgaris, Callogonum affilium, collected in the territory of Akmola region (Artemisia terra-albae, Thymus vulgaris) and Western Kazakhstan (Callogonum affilium). The first stage was the production of ethanol extracts of Artemisia terraea-albae, Thymus vulgaris, Callogonum affilium. To obtain them, 100 g of vegetable raw materials were taken, which was dissolved in 70% ethyl alcohol. Extraction was carried out for 2 hours at the boiling point of the solvent with a reverse refrigerator using an ultrasonic bath "Sapphire". The obtained extracts were evaporated on a rotary evaporator IKA RV 10. At the second stage, the three samples obtained were tested for antimicrobial and antifungal activity. Extracts of Thymus vulgaris and Callogonum affilium showed high antimicrobial and antifungal activity. Artemisia terraea-albae extract showed high antimicrobial activity and low antifungal activity. When testing method 1, it was found that in the first and third experimental groups there was a decrease in the concentration of aflatoxin B1 in walnut samples by 63 and 65%, respectively, but these values also exceeded the maximum permissible concentrations, while the nuts in the second and third experimental groups had a tart lemon flavor; When testing method 2, a decrease in the concentration of aflatoxin B1 to a safe level was observed by 91% (0.0038 mg/kg) in nuts of the 1st and 2nd experimental groups (Artemisia terra-albae, Thymus vulgaris), while in samples of the 2nd and 3rd experimental groups, a decrease in the amount of aflatoxin in 1 to a safe level was observed.

Keywords: nuts, aflatoxin B1, my, mycotoxins

Procedia PDF Downloads 56

Authors: Olga Gomez De Miranda, Jose R. Ochoa-Gomez, Stefaan De Wildeman, Luciano Monsegue, Soraya Prieto, Leire Lorenzo, Cristina Dineiro

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The chemical industry is facing a new revolution. As long as processes based on the exploitation of fossil resources emerged with force in the XIX century, Society currently demands a new radical change that will lead to the complete and irreversible implementation of a circular sustainable economic model. The implementation of biorefineries will be essential for this. There, renewable raw materials as sugars and other biomass resources are exploited for the development of new materials that will partially replace their petroleum-derived homologs in a safer, and environmentally more benign approach. Isosorbide, (1,4:3,6-dianhydro-d-glucidol) is a primary bio-based derivative obtained from the plant (poly) saccharides and a very interesting example of a useful chemical produced in biorefineries. It can, in turn, be converted to other secondary monomers as isosorbide bis-methyl carbonate (IBMC), whose main field of application can be as a key biodegradable intermediary substitute of bisphenol-A in the manufacture of polycarbonates, or as an alternative to the toxic isocyanates in the synthesis of new polyurethanes (non-isocyanate polyurethanes) both with a huge application market. New products will present advantageous mechanical or optical properties, as well as improved behavior in non-toxicity and biodegradability aspects in comparison to their petro-derived alternatives. A robust production process of IBMC, a biomass-derived chemical, is here presented. It can be used with different raw material qualities using dimethyl carbonate (DMC) as both co-reactant and solvent. It consists of the transesterification of isosorbide with DMC under soft operational conditions, using different basic catalysts, always active with the isosorbide characteristics and purity. Appropriate isolation processes have been also developed to obtain crude IBMC yields higher than 90%, with oligomers production lower than 10%, independently of the quality of the isosorbide considered. All of them are suitable to be used in polycondensation reactions for polymers obtaining. If higher qualities of IBMC are needed, a purification treatment based on nanofiltration membranes has been also developed. The IBMC reaction-isolation conditions established in the laboratory have been successfully modeled using appropriate software programs and moved to a pilot-scale (production of 100 kg of IBMC). It has been demonstrated that a highly efficient IBMC production process able to be up-scaled under suitable market conditions has been obtained. Operational conditions involved the production of IBMC involve soft temperature and energy needs, no additional solvents, and high operational efficiency. All of them are according to green manufacturing rules.

Keywords: biomass, catalyst, isosorbide bis-methyl carbonate, polycarbonate, polyurethane, transesterification

Procedia PDF Downloads 104

Authors: Choy Sonny Yip Hong

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This abstract presents an exploration into the creation of a sustainable bio-polymer compound for additive manufacturing, specifically 3D printing, with a focus on eggshells and polylactide (PLA) polymer. The project initially conducted experiments using a variety of food by-products to create bio-polymers, and promising results were obtained when combining eggshells with PLA polymer. The research journey involved precise measurements, drying of PLA to remove moisture, and the utilization of a filament-making machine to produce 3D printable filaments. The project began with exploratory research and experiments, testing various combinations of food by-products to create bio-polymers. After careful evaluation, it was discovered that eggshells and PLA polymer produced promising results. The initial mixing of the two materials involved heating them just above the melting point. To make the compound 3D printable, the research focused on finding the optimal formulation and production process. The process started with precise measurements of the PLA and eggshell materials. The PLA was placed in a heating oven to remove any absorbed moisture. Handmade testing samples were created to guide the planning for 3D-printed versions. The scrap PLA was recycled and ground into a powdered state. The drying process involved gradual moisture evaporation, which required several hours. The PLA and eggshell materials were then placed into the hopper of a filament-making machine. The machine's four heating elements controlled the temperature of the melted compound mixture, allowing for optimal filament production with accurate and consistent thickness. The filament-making machine extruded the compound, producing filament that could be wound on a wheel. During the testing phase, trials were conducted with different percentages of eggshell in the PLA mixture, including a high percentage (20%). However, poor extrusion results were observed for high eggshell percentage mixtures. Samples were created, and continuous improvement and optimization were pursued to achieve filaments with good performance. To test the 3D printability of the DIY filament, a 3D printer was utilized, set to print the DIY filament smoothly and consistently. Samples were printed and mechanically tested using a universal testing machine to determine their mechanical properties. This testing process allowed for the evaluation of the filament's performance and suitability for additive manufacturing applications. In conclusion, the project explores the creation of a sustainable bio-polymer compound using eggshells and PLA polymer for 3D printing. The research journey involved precise measurements, drying of PLA, and the utilization of a filament-making machine to produce 3D printable filaments. Continuous improvement and optimization were pursued to achieve filaments with good performance. The project's findings contribute to the advancement of additive manufacturing, offering opportunities for design innovation, carbon footprint reduction, supply chain optimization, and collaborative potential. The utilization of eggshell PLA polymer in additive manufacturing has the potential to revolutionize the manufacturing industry, providing a sustainable alternative and enabling the production of intricate and customized products.

Keywords: additive manufacturing, 3D printing, eggshell PLA polymer, design innovation, carbon footprint reduction, supply chain optimization, collaborative potential

Procedia PDF Downloads 40

Authors: Sankha Chakrabortty, Biswajit Ruj, Parimal Pal

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Methanol is one of the most important chemical products and intermediates. It can be used as a solvent, intermediate or raw material for a number of higher valued products, fuels or additives. From the last one decay, the total global demand of methanol has increased drastically which forces the scientists to produce a large amount of methanol from a renewable source to meet the global demand with a sustainable way. Different types of non-renewable based raw materials have been used for the synthesis of methanol on a large scale which makes the process unsustainable. In this circumstances, photocatalytic conversion of CO₂ into methanol under solar/UV excitation becomes a viable approach to give a sustainable production approach which not only meets the environmental crisis by recycling CO₂ to fuels but also reduces CO₂ amount from the atmosphere. Development of such sustainable production approach for CO₂ conversion into methanol still remains a major challenge in the current research comparing with conventional energy expensive processes. In this backdrop, the development of environmentally friendly materials, like photocatalyst has taken a great perspective for methanol synthesis. Scientists in this field are always concerned about finding an improved photocatalyst to enhance the photocatalytic performance. Graphene-based hybrid and composite materials with improved properties could be a better nanomaterial for the selective conversion of CO₂ to methanol under visible light (solar energy) or UV light. The present invention relates to synthesis an improved heterogeneous graphene-based photocatalyst with improved catalytic activity and surface area. Graphene with enhanced surface area is used as coupled material of copper-loaded titanium oxide to improve the electron capture and transport properties which substantially increase the photoinduced charge transfer and extend the lifetime of photogenerated charge carriers. A fast reduction method through H₂ purging has been adopted to synthesis improved graphene whereas ultrasonication based sol-gel method has been applied for the preparation of graphene coupled copper loaded titanium oxide with some enhanced properties. Prepared photocatalysts were exhaustively characterized using different characterization techniques. Effects of catalyst dose, CO₂ flow rate, reaction temperature and stirring time on the efficacy of the system in terms of methanol yield and productivity have been studied in the present study. The study shown that the newly synthesized photocatalyst with an enhanced surface resulting in a sustained productivity and yield of methanol 0.14 g/Lh, and 0.04 g/gcat respectively, after 3 h of illumination under UV (250W) at an optimum catalyst dosage of 10 g/L having 1:2:3 (Graphene: TiO₂: Cu) weight ratio.

Keywords: renewable energy, CO₂ capture, photocatalytic conversion, methanol

Procedia PDF Downloads 89

Authors: Anton G. Kalmykov, Andrew Yu. Bychkov, Georgy A. Kalmykov

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Nowadays, most oil reserves in Russia and all over the world are hard to recover. That is the reason oil companies are searching for new sources for hydrocarbon production. One of the sources might be high-carbon formations with unconventional reservoirs. Bazhenov formation is a huge source rock formation located in West Siberia, which contains unconventional reservoirs on some of the areas. These reservoirs are formed by secondary processes with low predicting ratio. Only one of five wells is drilled through unconventional reservoirs, in others kerogen has low thermal maturity, and they are of low petroliferous. Therefore, there was a request for tertiary methods for in-situ cracking of kerogen and production of oil. Laboratory experiments of Bazhenov formation rock hydrous pyrolysis were used to investigate features of the oil generation process. Experiments on Bazhenov rocks with a different mineral composition (silica concentration from 15 to 90 wt.%, clays – 5-50 wt.%, carbonates – 0-30 wt.%, kerogen – 1-25 wt.%) and thermal maturity (from immature to late oil window kerogen) were performed in a retort under reservoir conditions. Rock samples of 50 g weight were placed in retort, covered with water and heated to the different temperature varied from 250 to 400°C with the durability of the experiments from several hours to one week. After the experiments, the retort was cooled to room temperature; generated hydrocarbons were extracted with hexane, then separated from the solvent and weighted. The molecular composition of this synthesized oil was then investigated via GC-MS chromatography Characteristics of rock samples after the heating was measured via the Rock-Eval method. It was found, that the amount of synthesized oil and its composition depending on the experimental conditions and composition of rocks. The highest amount of oil was produced at a temperature of 350°C after 12 hours of heating and was up to 12 wt.% of initial organic matter content in the rocks. At the higher temperatures and within longer heating time secondary cracking of generated hydrocarbons occurs, the mass of produced oil is lowering, and the composition contains more hydrocarbons that need to be recovered by catalytical processes. If the temperature is lower than 300°C, the amount of produced oil is too low for the process to be economically effective. It was also found that silica and clay minerals work as catalysts. Selection of heating conditions allows producing synthesized oil with specified composition. Kerogen investigations after heating have shown that thermal maturity increases, but the yield is only up to 35% of the maximum amount of synthetic oil. This yield is the result of gaseous hydrocarbons formation due to secondary cracking and aromatization and coaling of kerogen. Future investigations will allow the increase in the yield of synthetic oil. The results are in a good agreement with theoretical data on kerogen maturation during oil production. Evaluated trends could be tooled up for in-situ oil generation by shale rocks thermal action.

Keywords: Bazhenov formation, fossil fuels, hydropyrolysis, synthetic oil

Procedia PDF Downloads 94

Authors: Andrea Dragu, Solen Kinayyigit, Valerie Colliere, Karin Karin Philippot, Camelia Bala, Vasile I. Parvulescu

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The production of transportation fuels from biomass has gained a growing attention due to diminishing fossil fuel reserves, rising petroleum prices and increasing concern about global warming. In recent years, renewable hydrocarbons that are completely fungible with fossil fuels have been suggested to be efficiently produced by catalytic deoxygenation of fatty acids and their derivatives viadecarboxylation / decarbonylation. Several triglycerides (tall oil fatty acids) and saturated/unsaturated fatty acids and their corresponding esters were used as feedstocks. Their impact together with the influence of the reaction conditions and the catalyst composition on the nature of the reaction pathways of the deoxygenation of vegetable oils and their derivatives were recently reviewed. Following this state of the art the aim of the present study was the investigation of Pd NPs deposited onto mesoporous carbon supports as active and stable catalysts for the deoxygenation of oleic acid. The catalysts were prepared by the deposition of Pd NPs synthesised following an organometallic route on mesoporous carbons with different characteristics. Experiments were carried out under both batch and flow conditions. They demonstrated that under batch conditions (200 atm; 573K), the extent of the reaction depended, firstly, on the Pd loading and then on the metal dispersion and the oxidation state of palladium, both influenced by the way the support has been treated before the NPs deposition and by the preparation/stabilization methodology of Pd NPs. No aromatic compounds were detected in the reaction products but octadecanol and octadecane were observed in large extents. Under flow conditions (4 atm; 573 K), the conversion of stearic acid was superior to that observed in batch conditions. The product mixture contained over 20% heptadecane. No octadecanol, octadecane, and aromatic compounds were detected. The maxima in performances are obtained after only 0.5 h. After that, the yields in heptadecane suffer from a severe decrease until 3h reaction time. However, at that time, stopping feeding the reactor with oleic acid and flushing the catalyst only with mesitylene recovered the activity and the selectivity of the catalysts. With the complete removal of H2, the analysis revealed the presence of heptadecene in high excess compared to heptadecane (almost 7 to 1), thus suggesting decarbonylation as the main route. ICP-OES measurements indicated no leaching of palladium and simple washing of catalysts with mesitylene allowed recycling without any change in conversion or product distribution. Noteworthy, mesitylene as solvent exhibited no effect in this reaction. In conclusion, this study demonstrates the feasibility of such catalysts for the green production of fuels from biomass.

Keywords: fuels from biomass, green catalyst, Pd nano-particles , recycble catalyst

Procedia PDF Downloads 283

Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

Procedia PDF Downloads 121

Authors: Ahmad S. Darwish, Tarek Lemaoui, Hanifa Taher, Inas M. AlNashef, Fawzi Banat

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This research reports a systematic top-down approach for designing neoteric hydrophobic solvents –particularly, deep eutectic solvents (DES) and ionic liquids (IL)– as furfural extractants from aqueous media for the application of sustainable biomass conversion. The first stage of the framework entailed screening 32 neoteric solvents to determine their efficacy against toluene as the application’s conventional benchmark for comparison. The selection criteria for the best solvents encompassed not only their efficiency in extracting furfural but also low viscosity and minimal toxicity levels. Additionally, for the DESs, their natural origins, availability, and biodegradability were also taken into account. From the screening pool, two neoteric solvents were selected: thymol:decanoic acid 1:1 (Thy:DecA) and trihexyltetradecyl phosphonium bis(trifluoromethylsulfonyl) imide [P₁₄,₆,₆,₆][NTf₂]. These solvents outperformed the toluene benchmark, achieving efficiencies of 94.1% and 97.1% respectively, compared to toluene’s 81.2%, while also possessing the desired properties. These solvents were then characterized thoroughly in terms of their physical properties, thermal properties, critical properties, and cross-contamination solubilities. The selected neoteric solvents were then extensively tested under various operating conditions, and an exceptional stable performance was exhibited, maintaining high efficiency across a broad range of temperatures (15–100 °C), pH levels (1–13), and furfural concentrations (0.1–2.0 wt%) with a remarkable equilibrium time of only 2 minutes, and most notably, demonstrated high efficiencies even at low solvent-to-feed ratios. The durability of the neoteric solvents was also validated to be stable over multiple extraction-regeneration cycles, with limited leachability to the aqueous phase (≈0.1%). Moreover, the extraction performance of the solvents was then modeled through machine learning, specifically multiple non-linear regression (MNLR) and artificial neural networks (ANN). The models demonstrated high accuracy, indicated by their low absolute average relative deviations with values of 2.74% and 2.28% for Thy:DecA and [P₁₄,₆,₆,₆][NTf₂], respectively, using MNLR, and 0.10% for Thy:DecA and 0.41% for [P₁₄,₆,₆,₆][NTf₂] using ANN, highlighting the significantly enhanced predictive accuracy of the ANN. The neoteric solvents presented herein offer noteworthy advantages over traditional organic solvents, including their high efficiency in both extraction and regeneration processes, their stability and minimal leachability, making them particularly suitable for applications involving aqueous media. Moreover, these solvents are more environmentally friendly, incorporating renewable and sustainable components like thymol and decanoic acid. This exceptional efficacy of the newly developed neoteric solvents signifies a significant advancement, providing a green and sustainable alternative for furfural production from biowaste.

Keywords: sustainable biomass conversion, furfural extraction, ionic liquids, deep eutectic solvents

Procedia PDF Downloads 39

Authors: Adeline Meriaux, Claire Gaiani, Jennifer Burgain, Frantz Fournier, Lionel Muniglia, Jérémy Petit

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Spray-drying process is widely used for the production of dairy powders for food and pharmaceuticals industries. It involves the atomization of a liquid feed into fine droplets, which are subsequently dried through contact with a hot air flow. The resulting powders permit transportation cost reduction and shelf life increase but can also exhibit various interesting functionalities (flowability, solubility, protein modification or acid gelation), depending on operating conditions and milk composition. Indeed, particles porosity, surface composition, lactose crystallization, protein denaturation, protein association or crust formation may change. Links between spray-drying conditions and physicochemical and functional properties of powders were investigated by a design of experiment methodology and analyzed by principal component analysis. Quadratic models were developed, and multicriteria optimization was carried out by the use of genetic algorithm. At the time of abstract submission, verification spray-drying trials are ongoing. To perform experiments, milk from dairy farm was collected, skimmed, froze and spray-dried at different air pressure (between 1 and 3 bars) and outlet temperature (between 75 and 95 °C). Dry matter, minerals content and proteins content were determined by standard method. Solubility index, absorption index and hygroscopicity were determined by method found in literature. Particle size distribution were obtained by laser diffraction granulometry. Location of the powder color in the Cielab color space and water activity were characterized by a colorimeter and an aw-value meter, respectively. Flow properties were characterized with FT4 powder rheometer; in particular compressibility and shearing test were performed. Air pressure and outlet temperature are key factors that directly impact the drying kinetics and powder characteristics during spray-drying process. It was shown that the air pressure affects the particle size distribution by impacting the size of droplet exiting the nozzle. Moreover, small particles lead to more cohesive powder and less saturated color of powders. Higher outlet temperature results in lower moisture level particles which are less sticky and can explain a spray-drying yield increase and the higher cohesiveness; it also leads to particle with low water activity because of the intense evaporation rate. However, it induces a high hygroscopicity, thus, powders tend to get wet rapidly if they are not well stored. On the other hand, high temperature provokes a decrease of native serum proteins which is positively correlated to gelation properties (gel point and firmness). Partial denaturation of serum proteins can improve functional properties of powder. The control of air pressure and outlet temperature during the spray-drying process significantly affects the physicochemical and functional properties of powder. This study permitted to better understand the links between physicochemical and functional properties of powder, to identify correlations between air pressure and outlet temperature. Therefore, mathematical models have been developed and the use of genetic algorithm will allow the optimization of powder functionalities.

Keywords: dairy powders, spray-drying, powders functionalities, design of experiment

Procedia PDF Downloads 52

Authors: Tatiana V. Melnikova, Lyudmila P. Polyakova, Alla A. Oudalova

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As a result of environmental pollution, the production of agriculture and foodstuffs inevitably contain residual amounts of Persistent Organic Pollutants (POP). The special attention must be given to organic pollutants, including various organochlorinated pesticides (OCP). Among priorities, OCP is DDT (and its metabolite DDE), alfa-HCH, gamma-HCH (lindane). The control of these substances spends proceeding from requirements of sanitary norms and rules. During too time often is lost sight of that the primary product can pass technological processing (in particular irradiation treatment) as a result of which transformation of physicochemical forms of initial polluting substances is possible. The goal of the present work was to study the OCP radiation degradation at a various gamma-radiation dosimetric characteristics. The problems posed for goal achievement: to evaluate the content of the priority of OCPs in food; study the character the degradation of OCP in model solutions (with micro concentrations commensurate with the real content of their agricultural and food products) depending upon dosimetric characteristics of gamma-radiation. Qualitative and quantitative analysis of OCP in food and model solutions by gas chromatograph Varian 3400 (Varian, Inc. (USA)); chromatography-mass spectrometer Varian Saturn 4D (Varian, Inc. (USA)) was carried out. The solutions of DDT, DDE, alpha- and gamma- isomer HCH (0.01, 0.1, 1 ppm) were irradiated on "Issledovatel" (60Co) and "Luch - 1" (60Co) installations at a dose 10 kGy with a variation of dose rate from 0.0083 up to 2.33 kGy/sec. It was established experimentally that OCP residual concentration in individual samples of food products (fish, milk, cereal crops, meat, butter) are evaluated as 10-1-10-4 mg/kg, the value of which depends on the factor-sensations territory and natural migration processes. The results were used in the preparation of model solutions OCP. The dependence of a degradation extent of OCP from a dose rate gamma-irradiation has complex nature. According to our data at a dose 10 kGy, the degradation extent of OCP at first increase passes through a maximum (over the range 0.23 – 0.43 Gy/sec), and then decrease with the magnification of a dose rate. The character of the dependence of a degradation extent of OCP from a dose rate is kept for various OCP, in polar and nonpolar solvents and does not vary at the change of concentration of the initial substance. Also in work conditions of the maximal radiochemical yield of OCP which were observed at having been certain: influence of gamma radiation with a dose 10 kGy, in a range of doses rate 0.23 – 0.43 Gy/sec; concentration initial OCP 1 ppm; use of solvent - 2-propanol after preliminary removal of oxygen. Based on, that at studying model solutions of OCP has been established that the degradation extent of pesticides and qualitative structure of OCP radiolysis products depend on a dose rate, has been decided to continue researches radiochemical transformations OCP into foodstuffs at various of doses rate.

Keywords: degradation extent, dosimetric characteristics, gamma-radiation, organochlorinated pesticides, persistent organic pollutants

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Authors: Kai-Cheng Yang, Yen-Ling Chen, Er-Chieh Cho, Kuen-Chan Lee

Abstract:

Titanium dioxide nanomaterials offer superior protection for human skin against the full spectrum of ultraviolet light. However, some literature reviews indicated that it might be associated with adverse effects such as cytotoxicity or reactive oxygen species (ROS) due to their nanoscale. The surface of fullerene is covered with π electrons constituting aromatic structures, which can effectively scavenge large amount of radicals. Unfortunately, fullerenes are poor solubility in water, severe aggregation, and toxicity in biological applications when dispersed in solvent have imposed the limitations to the use of fullerenes. Carboxyfullerene acts as the scavenger of radicals for several years. Some reports indicate that carboxyfullerene not only decrease the concentration of free radicals in ambience but also prevent cells from reducing the number or apoptosis under UV irradiation. The aim of this study is to decorate fullerene –C70-carboxylic acid (C70-COOH) on the surface of titanium dioxide nanoparticles (P25) for the purpose of scavenging ROS during the irradiation. The modified material is prepared through the esterification of C70-COOH with P25 (P25/C70-COOH). The binding edge and structure are studied by using Transmission electron microscope (TEM) and Fourier transform infrared (FTIR). The diameter of P25 is about 30 nm and C70-COOH is found to be conjugated on the edge of P25 in aggregation morphology with the size of ca. 100 nm. In the next step, the FTIR was used to confirm the binding structure between P25 and C70-COOH. There are two new peaks are shown at 1427 and 1720 cm-1 for P25/C70-COOH, resulting from the C–C stretch and C=O stretch formed during esterification with dilute sulfuric acid. The IR results further confirm the chemically bonded interaction between C70-COOH and P25. In order to provide the evidence of scavenging radical ability of P25/C70-COOH, we chose pyridoxine (Vit.B6) and terephthalic acid (TA) to react with singlet oxygen and hydroxyl radicals. We utilized these chemicals to observe the radicals scavenging statement via detecting the intensity of ultraviolet adsorption or fluorescence emission. The UV spectra are measured by using different concentration of C70-COOH modified P25 with 1mM pyridoxine under UV irradiation for various duration times. The results revealed that the concentration of pyridoxine was increased when cooperating with P25/C70-COOH after three hours as compared with control (only P25). It indicates fewer radicals could be reacted with pyridoxine because of the absorption via P25/C70-COOH. The fluorescence spectra are observed by measuring P25/C70-COOH with 1mM terephthalic acid under UV irradiation for various duration times. The fluorescence intensity of TAOH was decreased in ten minutes when cooperating with P25/C70-COOH. Here, it was found that the fluorescence intensity was increased after thirty minutes, which could be attributed to the saturation of C70-COOH in the absorption of radicals. However, the results showed that the modified P25/C70-COOH could reduce the radicals in the environment. Therefore, we expect that P25/C70-COOH is a potential materials in using for antioxidant.

Keywords: titanium dioxide, fullerene, radical scavenging activity, antioxidant

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Authors: N. Szczepanska, B. Kudlak, G. Yotova, S. Tsakovski, J. Namiesnik

Abstract:

In the scientific literature related to the widely understood issue of packaging materials designed to have contact with food (food contact materials), there is much information on raw materials used for their production, as well as their physiochemical properties, types, and parameters. However, not much attention is given to the issues concerning migration of toxic substances from packaging and its actual influence on the health of the final consumer, even though health protection and food safety are the priority tasks. The goal of this study was to estimate the impact of particular foodstuff packaging type, food production, and storage conditions on the degree of leaching of potentially toxic compounds and endocrine disruptors to foodstuffs using the acute toxicity test Microtox and XenoScreen YES YAS assay. The selected foodstuff packaging materials were metal cans used for fish storage and tetrapak. Five stimulants respectful to specific kinds of food were chosen in order to assess global migration: distilled water for aqueous foods with a pH above 4.5; acetic acid at 3% in distilled water for acidic aqueous food with pH below 4.5; ethanol at 5% for any food that may contain alcohol; dimethyl sulfoxide (DMSO) and artificial saliva were used in regard to the possibility of using it as an simulation medium. For each packaging three independent variables (temperature and contact time) factorial design simulant was performed. Xenobiotics migration from epoxy resins was studied at three different temperatures (25°C, 65°C, and 121°C) and extraction time of 12h, 48h and 2 weeks. Such experimental design leads to 9 experiments for each food simulant as conditions for each experiment are obtained by combination of temperature and contact time levels. Each experiment was run in triplicate for acute toxicity and in duplicate for estrogen disruption potential determination. Multi-factor analysis of variation (MANOVA) was used to evaluate the effects of the three main factors solvent, temperature (temperature regime for cup), contact time and their interactions on the respected dependent variable (acute toxicity or estrogen disruption potential). From all stimulants studied the most toxic were can and tetrapak lining acetic acid extracts that are indication for significant migration of toxic compounds. This migration increased with increase of contact time and temperature and justified the hypothesis that food products with low pH values cause significant damage internal resin filling. Can lining extracts of all simulation medias excluding distilled water and artificial saliva proved to contain androgen agonists even at 25°C and extraction time of 12h. For tetrapak extracts significant endocrine potential for acetic acid, DMSO and saliva were detected.

Keywords: food packaging, extraction, migration, toxicity, biotest

Procedia PDF Downloads 160

Authors: S. Ebadzadsahraei, H. Kazemian

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The main objective of this research was to measure particulate matter (PM₂.₅) and Volatile Organic Compound (VOCs) as two classes of air pollutants, at Prince George (PG) neighborhood in warm and cold seasons. To fulfill this objective, analytical protocols were developed for accurate sampling and measurement of the targeted air pollutants. PM₂.₅ samples were analyzed for their chemical composition (i.e., toxic trace elements) in order to assess their potential source of emission. The City of Prince George, widely known as the capital of northern British Columbia (BC), Canada, has been dealing with air pollution challenges for a long time. The city has several local industries including pulp mills, a refinery, and a couple of asphalt plants that are the primary contributors of industrial VOCs. In this research project, which is the first study of this kind in this region it measures physical and chemical properties of particulate air pollutants (PM₂.₅) at the city neighborhood. Furthermore, this study quantifies the percentage of VOCs at the city air samples. One of the outcomes of this project is updated data about PM₂.₅ and VOCs inventory in the selected neighborhoods. For examining PM₂.₅ chemical composition, an elemental analysis methodology was developed to measure major trace elements including but not limited to mercury and lead. The toxicity of inhaled particulates depends on both their physical and chemical properties; thus, an understanding of aerosol properties is essential for the evaluation of such hazards, and the treatment of such respiratory and other related diseases. Mixed cellulose ester (MCE) filters were selected for this research as a suitable filter for PM₂.₅ air sampling. Chemical analyses were conducted using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for elemental analysis. VOCs measurement of the air samples was performed using a Gas Chromatography-Flame Ionization Detector (GC-FID) and Gas Chromatography-Mass Spectrometry (GC-MS) allowing for quantitative measurement of VOC molecules in sub-ppb levels. In this study, sorbent tube (Anasorb CSC, Coconut Charcoal), 6 x 70-mm size, 2 sections, 50/100 mg sorbent, 20/40 mesh was used for VOCs air sampling followed by using solvent extraction and solid-phase micro extraction (SPME) techniques to prepare samples for measuring by a GC-MS/FID instrument. Air sampling for both PM₂.₅ and VOC were conducted in summer and winter seasons for comparison. Average concentrations of PM₂.₅ are very different between wildfire and daily samples. At wildfire time average of concentration is 83.0 μg/m³ and daily samples are 23.7 μg/m³. Also, higher concentrations of iron, nickel and manganese found at all samples and mercury element is found in some samples. It is able to stay too high doses negative effects.

Keywords: air pollutants, chemical analysis, particulate matter (PM₂.₅), volatile organic compound, VOCs

Procedia PDF Downloads 116

Authors: Adeline Meriaux, Claire Gaiani, Jennifer Burgain, Frantz Fournier, Lionel Muniglia, Jérémy Petit

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Spray-drying process is widely used for the production of dairy powders for food and pharmaceuticals industries. It involves the atomization of a liquid feed into fine droplets, which are subsequently dried through contact with a hot air flow. The resulting powders permit transportation cost reduction and shelf life increase but can also exhibit various interesting functionalities (flowability, solubility, protein modification or acid gelation), depending on operating conditions and milk composition. Indeed, particles porosity, surface composition, lactose crystallization, protein denaturation, protein association or crust formation may change. Links between spray-drying conditions and physicochemical and functional properties of powders were investigated by a design of experiment methodology and analyzed by principal component analysis. Quadratic models were developed, and multicriteria optimization was carried out by the use of genetic algorithm. At the time of abstract submission, verification spray-drying trials are ongoing. To perform experiments, milk from dairy farm was collected, skimmed, froze and spray-dried at different air pressure (between 1 and 3 bars) and outlet temperature (between 75 and 95 °C). Dry matter, minerals content and proteins content were determined by standard method. Solubility index, absorption index and hygroscopicity were determined by method found in literature. Particle size distribution were obtained by laser diffraction granulometry. Location of the powder color in the Cielab color space and water activity were characterized by a colorimeter and an aw-value meter, respectively. Flow properties were characterized with FT4 powder rheometer; in particular, compressibility and shearing test were performed. Air pressure and outlet temperature are key factors that directly impact the drying kinetics and powder characteristics during spray-drying process. It was shown that the air pressure affects the particle size distribution by impacting the size of droplet exiting the nozzle. Moreover, small particles lead to more cohesive powder and less saturated color of powders. Higher outlet temperature results in lower moisture level particles which are less sticky and can explain a spray-drying yield increase and the higher cohesiveness; it also leads to particle with low water activity because of the intense evaporation rate. However, it induces a high hygroscopicity, thus, powders tend to get wet rapidly if they are not well stored. On the other hand, high temperature provokes a decrease of native serum proteins, which is positively correlated to gelation properties (gel point and firmness). Partial denaturation of serum proteins can improve functional properties of powder. The control of air pressure and outlet temperature during the spray-drying process significantly affects the physicochemical and functional properties of powder. This study permitted to better understand the links between physicochemical and functional properties of powder to identify correlations between air pressure and outlet temperature. Therefore, mathematical models have been developed, and the use of genetic algorithm will allow the optimization of powder functionalities.

Keywords: dairy powders, spray-drying, powders functionalities, design of experiment

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Authors: Feiyu Yang, Chunfang Ni, Rong Wang, Yun Zou, Wenbin Liu, Chenggong Zhang, Fenjin Sun, Chun Wang

Abstract:

Cocaine is the most frequently used illegal drug globally, with the global annual prevalence of cocaine used ranging from 0.3% to 0.4 % of the adult population aged 15–64 years. Growing consumption trend of abused cocaine and drug crimes are a great concern, therefore urine sample testing has become an important noninvasive sampling whereas cocaine and its metabolites (COCs) are usually present in high concentrations and relatively long detection windows. However, direct analysis of urine samples is not feasible because urine complex medium often causes low sensitivity and selectivity of the determination. On the other hand, presence of low doses of analytes in urine makes an extraction and pretreatment step important before determination. Especially, in gathered taking drug cases, the pretreatment step becomes more tedious and time-consuming. So developing a sensitive, rapid and high-throughput method for detection of COCs in human body is indispensable for law enforcement officers, treatment specialists and health officials. In this work, a new automated magnetic dispersive solid-phase extraction (MDSPE) sampling method followed by high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for quantitative enrichment of COCs from human urine, using prepared magnetic nanoparticles as absorbants. The nanoparticles were prepared by silanizing magnetic Fe3O4 nanoparticles and modifying them with divinyl benzene and vinyl pyrrolidone, which possesses the ability for specific adsorption of COCs. And this kind of magnetic particle facilitated the pretreatment steps by electromagnetically controlled extraction to achieve full automation. The proposed device significantly improved the sampling preparation efficiency with 32 samples in one batch within 40mins. Optimization of the preparation procedure for the magnetic nanoparticles was explored and the performances of magnetic nanoparticles were characterized by scanning electron microscopy, vibrating sample magnetometer and infrared spectra measurements. Several analytical experimental parameters were studied, including amount of particles, adsorption time, elution solvent, extraction and desorption kinetics, and the verification of the proposed method was accomplished. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.1 ng·mL-1 with recoveries ranging from 75.1 to 105.7%. Compared to traditional sampling method, this method is time-saving and environmentally friendly. It was confirmed that the proposed automated method was a kind of highly effective way for the trace cocaine and cocaine metabolites analyses in human urine.

Keywords: automatic magnetic dispersive solid-phase extraction, cocaine detection, magnetic nanoparticles, urine sample testing

Procedia PDF Downloads 177