Search results for: headspace gas chromatography

Authors: D. S. Fardhyanti, A. Damayanti

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The utilization of biomass as a source of new and renewable energy is being carried out. One of the technologies to convert biomass as an energy source is pyrolysis which is converting biomass into more valuable products, such as bio-oil. Bio-oil is a liquid which is produced by steam condensation process from the pyrolysis of coconut shells. The composition of a coconut shell e.g. hemicellulose, cellulose and lignin will be oxidized to phenolic compounds as the main component of the bio-oil. The phenolic compounds in bio-oil are corrosive; they cause various difficulties in the combustion system because of a high viscosity, low calorific value, corrosiveness, and instability. Phenolic compounds are very valuable components which phenol has used as the main component for the manufacture of antiseptic, disinfectant (known as Lysol) and deodorizer. The experiments typically occurred at the atmospheric pressure in a pyrolysis reactor at temperatures ranging from 300 ^oC to 350 ^oC with a heating rate of 10 ^oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the bio-oil components. The obtained bio-oil has the viscosity of 1.46 cP, the density of 1.50 g/cm³, the calorific value of 16.9 MJ/kg, and the molecular weight of 1996.64. By GC-MS, the analysis of bio-oil showed that it contained phenol (40.01%), ethyl ester (37.60%), 2-methoxy-phenol (7.02%), furfural (5.45%), formic acid (4.02%), 1-hydroxy-2-butanone (3.89%), and 3-methyl-1,2-cyclopentanedione (2.01%).

Keywords: bio-oil, pyrolysis, coconut shell, phenol, gas chromatography-mass spectroscopy

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Authors: Tariq Ahmad Dar, Moinuddin, M. Masroor A. Khan

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There is considerable need in enhancing the content and yield of active constituents of medicinal plants keeping in view their massive demand worldwide. Different strategies have been employed to enhance the active constituents of medicinal plants and the use of phytohormones has been proved effective in this regard. Gamma-irradiated Sodium alginate (ISA) is known to elicit an array of plant defense responses and biological activities in plants. Considering the medicinal importance, a pot experiment was conducted to explore the effect of ISA and phosphorus on growth, yield and quality of fenugreek (Trigonella foenum-graecum L.). ISA spray treatments (0, 40, 80 and 120 mg L-1) were applied alone and in combination with 40 kg P ha-1 (P40). Crop performance was assessed in terms of plant growth characteristics, physiological attributes, seed yield and the content of seed trigonelline. Of the ten-treatments, P40 + 80 mg L−1 of ISA proved the best. The results showed that foliar spray of ISA alone or in combination with P40 augmented the plant vegetative growth, enzymatic activities, trigonelline content, trigonelline yield and economic yield of fenugreek. Application of 80 mg L−1 of ISA applied with P40 gave the best results for almost all the parameters studied compared to control or to 80 mg L−1 of ISA applied alone. This treatment increased the total content of chlorophyll, carotenoids, leaf -N, -P and -K and trigonelline compared to the control by 24.85 and 27.40%, 15 and 23.52%, 18.70 and 16.84%, 15.88 and 18.92%, 12 and 14.44%, at 60 and 90 DAS respectively. The combined application of 80 mg L−1 of ISA along with P40 resulted in the maximum increase in seed yield, trigonelline content and trigonelline yield by146, 34 and 232.41%, respectively, over the control. Gel permeation chromatography revealed the formation of low molecular weight fractions in ISA samples, containing even less than 20,000 molecular weight oligomers, which might be responsible for plant growth promotion in this study. Trigonelline content was determined by reverse phase high performance liquid chromatography (HPLC) with C-18 column.

Keywords: gamma-irradiated sodium alginate, phosphorus, gel permeation chromatography, HPLC, trigonelline content, yield

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Authors: Hye Rim Kang, So Yae Koh, Ji-Yeon Ryu, Chang Kyu Lee, Ji Hee Lim, Hyeon A. Kim, Geun Hyung Im, Somi Kim Cho

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In this study, antioxidant properties and compositional analysis of fermented chocolate were examined. Chocolate was fermented with Lactobacillus plantarum CK10. As fermentation time went by, pH was decreased (5.26±0.02 to 3.98±0.06) while titratable acidity was increased (5.36±0.19 to 13.31±0.34). The total polyphenol contents were maintained through the fermentation. The contents of total polyphenol were slightly increased at 8 hr (6.34±0.12 mg GAE (Gallic acid equivalent)/g), and it reached to comparable levels of the control at 24 hr (control, 5.47±0.36 mg GAE/g); 24 hr, 5.19±0.23 mg GAE/g). Similarly, the total flavonoid contents were not significantly changed during fermentation. The pronounced radical scavenging activities of chocolate, against DPPH-, ABTS-, and Alkyl radical, were observed. The levels of antioxidant activities were not dramatically altered in the course of fermentation. By gas chromatography-mass spectrometry analysis, the increase in lactic acid was measured and four major compounds, HMF, xanthosine, caffeine, and theobromine, were identified. The relative peak area of caffeine and theobromine was considerably changed during fermentation. However, no significant difference in the levels of caffeine and theobromine were observed by high-performance liquid chromatography analysis.

Keywords: antioxidant, chocolate, compositional analysis, fermentation, Lactobaillus plantarum

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Authors: Espinoza S. Clara, Gamarra Q. Flor, Marianela F. Ramos Quispe S. Miguel, Flores R. Omar

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Tropaeolum majus L. is a native plant to South and Central America, used since ancient times by our ancestors to combat different diseases. Glucotropaeolonin is one of its main components, which when hydrolyzed, forms benzyl isothiocyanate (BIT) that promotes cellular apoptosis (programmed cell death in cancer cells). Therefore, the present research aims to evaluate the effect of the pressure and temperature of BIT extraction by supercritical CO₂ from Tropaeolum majus L. The extraction was carried out in a supercritical fluid extractor equipment Speed SFE BASIC Brand: Poly science, the leaves of Tropaeolum majus L. were ground for one hour and lyophilized until obtaining a humidity of 6%. The extraction with supercritical CO₂ was carried out with pressures of 200 bar and 300 bar, temperatures of 50°C, 60°C and 70°C, obtained by the conjugation of these six treatments. BIT was identified by thin layer chromatography using 98% BIT as the standard, and as the mobile phase hexane: dichloromethane (4:2). Subsequently, BIT quantification was performed by high performance liquid chromatography (HPLC). The highest yield of oleoresin by supercritical CO₂ extraction was obtained pressure 300 bar and temperature at 60°C; and the higher content of BIT at pressure 200 bar and 70°C for 30 minutes to obtain 113.615 ± 0.03 mg BIT/100 g dry matter was obtained.

Keywords: solvent extraction, Tropaeolum majus L., supercritical fluids, benzyl isothiocyanate

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Authors: Rosemary Anibogwu, Kavita Sharma, Karl De Jesus

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Sagebrush is an abundant and naturally occurring plant in the Intermountain West region of the United States. The plant contains an array of bioactive compounds such as flavonoids, terpenoids, sterols, and phenolic acids. It is important to identify and characterize these compounds because Native Americans use sagebrush as herbal medicine. These compounds are also utilized for preventing infection in wounds, treating headaches and colds, and possess antitumor properties. This research is an exploratory study on the sesquiterpene present in the leaves of sagebrush. The leaf foliage was extracted with 100 % chloroform and 100 % methanol. The percentage yield for the crude was considerably higher in chloroform. The Thin Layer Chromatography (TLC) analysis of the crude extracted unveiled a brown band at Rf = 0.25 and a dark brown band at Rf = 0.74, along with three unknown faint bands the 254 nm UV lamp. Furthermore, the two distinct brown (Achillin) and dark brown band (Hydroxyachillin) in TLC were further utilized in the isolation of pure compounds with column chromatography. The structures of Achillin and Hydroxyachillin were elucidated based on extensive spectroscopic analysis, including TLC, High-Performance Liquid Chromatography (HPLC), 1D- and 2D-Nuclear Magnetic Resonance (NMR), and Mass Spectroscopy (MS). The antioxidant activities of crude extract and three pure compounds were evaluated in terms of their peroxyl radical scavenging by Ferric Reducing Ability of Plasma (FRAP) and 1,1-Diphenyl-2-picryl-hydrazyl (DPPH) methods. The crude extract showed the antioxidant activity of 18.99 ± 0.51 µmol TEg -1 FW for FRAP and 11.59 ± 0.38 µmol TEg -1 FW for DPPH. The activities of Achillin, Hydroxyachillin, and Quercetagetin trimethyl ether were 13.03, 15.90 and 14.02 µmol TEg -1 FW respectively for the FRAP assay. The three purified compounds have been submitted to the National Cancer Institute 60 cancer cell line for further study.

Keywords: HPLC, nuclear magnetic resonance spectroscopy, sagebrush, sesquiterpene lactones

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Authors: Lourena M. Veríssimo, Lucas A. Machado, Renata Rutckeviski, Francisco H. Xavier Júnior, Éverton N. Alencar, Andreza R. V. Morais, Teresa R. F. Dantas, Christian M. Oliveira, Arnóbio A. Silva Júnior, Eryvaldo S. T. Egito

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This study aimed to obtain emulsion systems based on bullfrog oil (BO). The BO was extracted at 80ºC and analyzed by Gas Chromatography-Mass Spectrometry (GC/MS). The critical Hydrophilic-Lipophilic Balance (HLBc) Assay of the BO was performed through BO, Tween® 20, Span® 80 and deionized water mixtures using an Ultra-Turrax® and determined using dynamic light scattering, pH, electrical conductivity and creaming rate. Then, a pseudoternary phase diagram (PPD) was constructed by water titration. The GC/MS analysis of BO suggested Methyl Oleate (9.26%) as major compound. The HLBc was 12.1, wherein the correspondent emulsion showed a pH of 4.83±1.29, electrical conductivity of 103.65 µS, creaming rate of 2.51±0.54%, droplet size of 207.07±8.31 nm and polydispersity index of 0.212±0.005. The PPD showed different formulations characterized as O/W emulsions. Thus, the PPD proved to be a useful tool to produce BO emulsions, in which their constituents may vary within the range of the desired system.

Keywords: bullfrog (Rana catesbeiana Shaw) oil, emulsion production, hydrophilic-lipophilic balance, gas chromatography/mass spectrometry analysis

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Authors: Donna M. Morrison, Lambert Chester, Coretta A. N. Samuels, David R. Ledoux

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A survey was conducted in the five rice-growing regions in Guyana to determine the presence of aflatoxins in multiple fractions of rice in June/October 2015 growing season. The fractions were paddy, steamed paddy, cargo rice, white rice and parboiled rice. Samples were analyzed by High Performance Liquid Chromatography. A subset of the samples was further analyzed by enzyme-linked immunosorbent assay (ELISA) for concurrence. All analyses were conducted at the University of Missouri, USA. Of the 186 samples tested, 16 had aflatoxin concentrations greater than 20 ppb the recommended limit for aflatoxins in food according to the United States Food and Drug Administration. An additional three samples had aflatoxin B₁ concentrations greater than the European Union Commission maximum levels for aflatoxin B₁ in rice at 5 µg/kg and total aflatoxins (B₁, B₂, G₁ and G₂) at 10 µg/kg. The survey indicates that there is no widespread aflatoxin problem in rice in Guyana. The incidence of aflatoxins appears to be localized.

Keywords: aflatoxin, enzyme-linked immunosorbent assay (ELISA), high-performance liquid chromatography (HPLC), rice fractions

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Authors: Milica Z. Karadzic, Lidija R. Jevric, Sanja Podunavac-Kuzmanovic, Strahinja Z. Kovacevic, Anamarija I. Mandic, Katarina Penov-Gasi, Andrea R. Nikolic, Aleksandar M. Okljesa

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In this study, a set of 29 newly synthesized steroid derivatives were investigated using reversed-phase high-performance liquid chromatography (RP-HPLC) as a first step in preselection of drug candidates. This analysis presents an experimental determination of chromatographic lipophilicity, and it was conducted to obtain physicochemical characterization of these molecules. As the most widely used bonded phases in RP-HPLC, octadecyl (C18) and octyl (C8) were used. Binary mixtures of water and acetonitrile or methanol were used as mobile phases. Obtained results were expressed as retention factor values logk and they were correlated with logP values. The results showed that both columns provide good estimations of the chromatographic lipophilicity of the molecules included in this study. This analysis was conducted in order to characterize newly synthesized steroid derivatives for further investigation regarding their antiproliferative and antimicrobial activity. This article is based upon work from COST Action (CM1306), supported by COST (European Cooperation in Science and Technology).

Keywords: antiproliferative activity, chromatographic lipophilicity, liquid chromatography, steroids

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Authors: Beena Sethi

Abstract:

This work involves the degradation of plastic waste in the presence of three different nanocatalysts. A thin film of LLDPE was formed with all three nanocatalysts separately in the solvent. Thermo Gravimetric Analysis (TGA) and Differential Scanning Calorimetric (DSC) analysis of polymers suggest that the presence of these catalysts lowers the degradation temperature and the change mechanism of degradation. Gas chromatographic analysis was carried out for two films. In gas chromatography (GC) analysis, it was found that degradation of pure polymer produces only 32% C3/C4 hydrocarbons and 67.6% C5/C9 hydrocarbons. In the presence of these catalysts, more than 80% of polymer by weight was converted into either liquid or gaseous hydrocarbons. Change in the mechanism of degradation of polymer was observed therefore more C3/C4 hydrocarbons along with valuable feedstock are produced. Adjustment of dose of nanocatalyst, use of nano-admixtures and recycling of catalyst can make this catalytic feedstock recycling method a good tool to get sustainable environment. The obtained products can be utilized as fuel or can be transformed into other useful products. In accordance with the principles of sustainable development, chemical recycling i.e. tertiary recycling of polymers along with the reuse (zero order recycling) of plastics can be the most appropriate and promising method in this direction. The tertiary recycling is attracting much attention from the viewpoint of the energy resource.

Keywords: degradation, differential scanning calorimetry, feedstock recycling, gas chromatography, thermogravimetric analysis

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Authors: Gokhan Zengin, Cengiz Sarikurkcu, Abdurrahman Aktumsek, Ramazan Ceylan

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The present study was designated to characterize the essential oil from S. galatica (SGEOs) and evaluate its antioxidant and enzyme inhibitory activities. Antioxidant capacity were tested different methods including free radical scavenging (DPPH, ABTS and NO), reducing power (FRAP and CUPRAC), metal chelating and phosphomolybdenum. Inhibitory activities were analyzed on acetylcholiesterase, butrylcholinesterase, α-amylase and α-glucosidase. SGEOs were chemically analyzed and identified by gas chromatography (GC) and gas chromatography/mass spectrophotometry (GC/MS). 23 components, representing 98.1% of SGEOs were identified. Monoterpene hydrocarbons (74.1%), especially α- (23.0%) and β-pinene (32.2%), were the main constituents in SGEOs. The main sesquiterpene hydrocarbons were β-caryophyllene (16.9%), Germacrene-D (1.2%) and Caryophyllene oxide (1.2%), respectively. Generally, SGEOs has shown moderate free radical, reducing power, metal chelating and enzyme inhibitory activities. These activities related to chemical profile in SGEOs. Our findings supported that the possible utility of SGEOs is a source of natural agents for food, cosmetics or pharmaceutical industries.

Keywords: sideritis galatica, antioxidant, monoterpenes, cholinesterase, anti-diabetic

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Authors: Jun Choi, Bo Ram Lee, Ji Hye Choi, Jung Soo Kim, No-Hyung Park, Dong Hyun Kim

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The synthetic rubber compound, which is widely used as the core material for automobile tire industry, is manufactured by mixing styrene-butadiene rubber (SBR) and organic/inorganic fillers. It is known that the most important factor for the physical properties of rubber compound is the interaction between the filler and the rubber, which affects the rotational, braking and abrasion resistance. Silica filler has hydrophilic groups such as a silanol group on their surface which has a low affinity with hydrophobic rubbers. In order to solve this problem, researches on an efficient silane coupling agent (SCA) has been continuously carried out. In this study, highly water-soluble SCAs which are expected to show higher hydrolysis efficiency were synthesized. The hydrophobization process of the silica with the prepared SCAs was economical and environment-friendly. The SCAs structures were analysed by gas chromatography-mass spectrometry (GC/MS) and nuclear magnetic resonance (1H-NMR) spectroscopy. In addition, their hydrolysis efficiency and condensation side reaction in SBR wet master batch were examined by Fourier transform infrared spectroscopy (FT-IR) and gel permeation chromatography (GPC), respectively.

Keywords: rubber, silane coupling agent, synthesis, water-soluble

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Authors: Sahira Nsayef Muslim, Israa M. S. Al-Kadmy, Nadheema Hammood Hussein, Alaa Naseer Mohammed Ali, Buthainah Mohammed Taha, Rayim Sabah Abbood, Sarah Naji Aziz

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A novel strain of Bacillus licheniformis isolated from spoilt cucumber and pepper samples have the ability to produce the chitosanase enzyme when grown on chitosan substrate. Chitosanase was purified to homogeneity with a recovery yield of 35.71% and 5.5 fold of purification by using ammonium sulfate at 45% saturation followed by ion exchange chromatography on DEAE-cellulose column and gel filtration chromatography on Sephadex G-100 column. The purified chitosanase inhibited the biofilm formation ability for all Gram-negative and Gram-positive biofilm-forming bacteria (biofilm producers) after using Congo Red agar and Microtiter plates methods. Highly antibiofilm of chitosanase recorded against Pseudomonas aeruginosa followed by Klebsiella pneumoniae with reduction of biofilm formation ratio to 22 and 29%, respectively compared with (100)% of control. Thus, chitosanase has promising benefit as antibiofilm agent against biofilm forming pathogenic bacteria and has promising application as alternative antibiofilm agents to combat the growing number of multidrug-resistant pathogen-associated infections, especially in situation where biofilms are involved.

Keywords: chitosanase, Bacillus licheniformis, vegetables, biofilm

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Authors: Niki K. Burns, James R. Pearson, Paul G. Stevenson, Xavier A. Conlan

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In Australian state Victoria, synthetic cannabinoids have recently been made illegal under an amendment to the drugs, poisons and controlled substances act 1981. Identification of synthetic cannabinoids in popular brands of ‘incense’ and ‘potpourri’ has been a difficult and challenging task due to the sample complexity and changes observed in the chemical composition of the cannabinoids of interest. This study has developed analytical methodology for the targeted extraction and determination of synthetic cannabinoids available pre-ban. A simple solvent extraction and solid phase extraction methodology was developed that selectively extracted the cannabinoid of interest. High performance liquid chromatography coupled with UV‐visible and chemiluminescence detection (acidic potassium permanganate and tris (2,2‐bipyridine) ruthenium(III)) were used to interrogate the synthetic cannabinoid products. Mass spectrometry and nuclear magnetic resonance spectroscopy were used for structural elucidation of the synthetic cannabinoids. The tris(2,2‐bipyridine)ruthenium(III) detection was found to offer better sensitivity than the permanganate based reagents. In twelve different brands of herbal incense, cannabinoids were extracted and identified including UR‐144, XLR 11, AM2201, 5‐F‐AKB48 and A796‐260.

Keywords: electrospray mass spectrometry, high performance liquid chromatography, solid phase extraction, synthetic cannabinoids

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Authors: Adesoji Sodeinde

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Analytical derivatives has recently undergone an explosive growth in areas of separation techniques, likewise in detectability of certain compound/concentrated ions. The gloomy and depressing scenario which charaterized the application of analytical derivatives in areas of water analysis, water cycle and the environment should not be allowed to continue unabated. Due to technological advancement in various chemical/biochemical analysis separation techniques is widely used in areas of medical, forensic and to measure and assesses environment and social-economic impact of alternative control strategies. This technological improvement was dully established in the area of comparison between certain separation/detection techniques to bring about vital result in forensic[as Gas liquid chromatography reveals the evidence given in court of law during prosecution of drunk drivers]. The water quality analysis,pH and water temperature analysis can be performed in the field, the concentration of dissolved free amino-acid [DFAA] can also be detected through separation techniques. Some important derivatives/ions used in separation technique. Water analysis : Total water hardness [EDTA to determine ca and mg ions]. Gas liquid chromatography : innovative gas such as helium [He] or nitrogen [N] Water cycle : Animal bone charcoal,activated carbon and ultraviolet light [U.V light].

Keywords: analytical derivative, environment, water analysis, chemical/biochemical analysis

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Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

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Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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Authors: Asmaa Mandour, Ramzia El-Bagary, Asmaa El-Zaher, Ehab Elkady

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Background: An UHPLC (ultra high performance liquid chromatography) method for the simultaneous determination of norfloxacin (NOR), metronidazole (MET) and tinidazole (TNZ) using monolithic column is presented. Purpose: The method is considered an environmentally friendly method with relatively low organic composition of the mobile phase. Methods: The chromatographic separation was performed using Phenomenex® Onyex Monolithic C18 (50mmx 20mm) column. An elution program of mobile phase consisted of 0.5% aqueous phosphoric acid : methanol (85:15, v/v). Where elution of all drugs was completed within 3.5 min with 1µL injection volume. The UHPLC method was applied for the stability indication of NOR in the presence of its acid degradation product ND. Results: Retention times were 0.69, 1.19 and 3.23 min for MET, TNZ and NOR, respectively. While ND retention time was 1.06 min. Linearity, accuracy, and precision were acceptable over the concentration range of 5-50µg mL-1for all drugs. Conclusions: The method is simple, sensitive and suitable for the routine quality control and dosage form assay of the three drugs and can also be used for the stability indication of NOR in the presence of its acid degradation product.

Keywords: antibacterial, monolithic cilumn, simultaneous determination, UHPLC

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Authors: O. E. Ogunjinmi, N. O. Olawore, L. A. Usman, S. O. Ogunjinmi

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An essential oil is any concentrated, hydrophobic liquid containing volatile aroma compounds produced by plants. It has been established that several factors affect the component of the plants such as the texture of the soil, relative humidity, wind, and collection time. This study is aimed at investigating the effect of collection time on the chemical composition of this essential oil. Pulverized leaves (500 g) of Hoslundia opposite harvested in the morning (7 am) and afternoon (2 pm) of the same day were separately hydrodistilled using Clevenger apparatus to obtain the essential oils from the leaves. The leaf oils collected in the morning (7 am) and afternoon (2 pm) harvests yielded 0.54 and 0.65 %w/w respectively. Analysis of the leaf oil obtained in the morning, using gas chromatography (GC) and gas chromatography combined mass spectrometry (GC-MS) revealed the presence of twenty-three (23) compounds which made up 81.8% of the total oil while nineteen (19) compounds (93.2%) were identified in the afternoon leaf essential oil. The most abundant components of the leaf oil collected in the morning (7 am) harvest were p-cymene (28.7%), sabinene (7.1%) and 1,8-cineole (6.6%) Meanwhile the major components of leaf oil in the afternoon (2 pm) harvest were p-cymene (26.4%), thymol (15.3%), 1,8-cineole (15.0%) and g-terpinene (10.4%). The composition pattern of leaf oil obtained in the morning and afternoon harvests of Hoslundia opposite revealed significant differences in qualitative and quantitative.

Keywords: essential oil, Hoslundia opposita, para cymene, 1, 8-cineole

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Authors: Sharareh Sharifi, Pargol Ghavam Mostafavi, Ali Mashinchian Moradi, Mohammad Hadi Givianrad, Hassan Niknejad

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Marine organisms such as soft coral, sponge, ascidians, and tunicate containing rich source of natural compound have been studied in last decades because of their special chemical compounds with anticancer properties. The aim of this study was to investigate anti-cancer property of ethyl acetate extracted from marine sea pen Virgularia gustaviana found from Persian Gulf coastal (Bandar Abbas). The extraction processes were carried out with ethyl acetate for five days. Thin layer chromatography (TLC) and high-performance liquid chromatography (HPLC) were used for qualitative identification of crude extract. The viability of HeLa and MDA-Mb-231 cancer cells was investigated using MTT assay at the concentration of 25, 50, and a 100 µl/ml of ethyl acetate is extracted. The crude extract of Virgularia gustaviana demonstrated ten fractions with different Retention factor (Rf) by TLC and Retention time (Rt) evaluated by HPLC. The crude extract dose-dependently decreased cancer cell viability compared to control group. According to the results, the ethyl acetate extracted from Virgularia gustaviana inhibits the growth of cancer cells, an effect which needs to be further investigated in the future studies.

Keywords: anti-cancer, Hela cancer cell, MDA-Md-231 cancer cell, Virgularia gustavina

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Authors: Mulatu Kassie Birhanu

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Electro-oxidation of glycerol is an important process to convert the less price glycerol into other expensive (essential) and energy-rich chemicals. In this study, nickel was electro-deposited on laboratory-made carbon ceramic electrode (CCE) substrate using electrochemical techniques that is cyclic voltammetry (CV) to prepare an electro-catalyst (Ni/CCE) for electro-oxidation of glycerol. Carbon ceramic electrode was prepared from graphite and methyl tri-methoxy silane (MTMOS) through the processes called hydrolysis and condensation with methanol in acidic media (HCl) by a sol-gel technique. Physico-chemical characterization of bare CCE and modified (deposited) CCE (Ni/CCE) was measured and evaluated by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). Electro-oxidation of glycerol was performed in 0.1 M glycerol in alkaline media (0.5 M NaOH). High-Performance Liquid Chromatography (HPLC) technique was used to identify and determine the concentration of glycerol, reaction intermediates and oxidized products of glycerol after its electro-oxidation is performed. The conversion (%) of electro-oxidation of glycerol during 9-hour oxidation was 73% and 36% at 1.8V and 1.6V vs. RHE, respectively. Formate, oxalate, glycolate and glycerate are the main oxidation products of glycerol with selectivity (%) of 75%, 8.6%, 1.1% and 0.95 % at 1.8 V vs. RHE and 55.4%, 2.2%, 1.0% and 0.6% at 1.6 V vs. RHE respectively. The result indicates that formate is the main product in the electro-oxidation of glycerol on Ni/CCE using the indicated applied potentials.

Keywords: carbon-ceramic electrode, electrodeposition, electro-oxidation, Methyltrimethoxysilane

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Authors: George Madalin Danila, Mihaiella Cretu, Cristian Puscasu

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Glycol-based anti-freeze liquids, commonly composed of ethylene glycol or propylene glycol, have important uses in automotive cooling, but they should be handled with care due to their toxicity; ethylene glycol is highly toxic to humans and animals. A fast, accurate, precise, and robust method was developed for the simultaneous quantification of 7 most important glycols and their isomers. Glycols were analyzed from diluted sample solution of coolants using gas-chromatography coupled with mass spectrometry in single ion monitoring mode. Results: The method was developed and validated for 7 individual glycols (ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol and tripropylene glycol). Limits of detection (1-2 μg/mL) and limit of quantification (10 μg/mL) obtained were appropriate. The present method was applied for the determination of glycols in 10 different anti-freeze liquids commercially available on the Romanian market, proving to be reliable. A method that requires only a two-step dilution of anti-freeze samples combined with direct liquid injection GC-MS was validated for the simultaneous quantification of 7 glycols (and their isomers) in 10 different types of anti-freeze liquids. The results obtained in the validation procedure proved that the GC-MS method is sensitive and precise for the quantification of glycols.

Keywords: glycols, anti-freeze, gas-chromatography, mass spectrometry, validation, recycle

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Authors: Yao-Te Yen, Chao-Hsin Cheng, Meng-Shun Huang, Shan-Zong Cyue

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'Poppy-seed defense' has been a serious problem all over the world, that is because the opiates metabolites in urine are difficult to distinguish where they come from precisely. In this research, a powerful analytic method has been developed to trace the opiates metabolites in urine by Gas-Chromatography Isotope Ratio Mass Spectrometry (GC-IRMS). In order to eliminate the interference of synthesis to heroin or metabolism through human body, opiates metabolites in urine and sized heroin were hydrolyzed to morphine. Morphine is the key compound for tracing between opiates metabolites and seized heroin in this research. By matching δ13C and δ15N values through morphine, it is successful to distinguish the opiates metabolites coming from heroin or medicine. We tested seven heroin abuser’s metabolites and seized heroin in crime sites, the result showed that opiates metabolites coming from seized heroin, the variation of δ13C and δ15N for morphine are within 0.2 and 2.5‰, respectively. The variation of δ13C and δ15N for morphine are reasonable with the result of matrix match experiments. Above all, the uncertainty of 'Poppy-seed defense' can be solved easily by this analytic method, it provides the direct evidence for judge to make accurate conviction without hesitation.

Keywords: poppy-seed defense, heroin, opiates metabolites, isotope ratio mass spectrometry

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Authors: Samy Selim

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Natural products are still major sources of innovative therapeutic agents for various conditions, including infectious diseases. Peganum harmala L. oil had wide range uses as traditional medicinal plants. The current study was designed to evaluate the antibacterial activity of P. harmala essential oil. The chemical constitutes and toxicity of these oils was also determined to obtain further information on the correlation between the chemical contents and antibacterial activity. The antibacterial effect of the essential oils of P. harmala oil was studied against some foodborne pathogenic bacteria species. The oil of plant was subjected to gas chromatography-mass spectrometry (GC/MS). The impact of oils administration on the change in rate of weight gain and complete blood picture in hamsters were investigated. P. harmala oil had strong antibacterial effect against bacterial species especially at minimum inhibitory concentration (MIC) less than 75.0 μg/ml. From the oil of P. harmala, forty one compounds were identified, and the major constituent was 1-hexyl-2-nitrocyclohexane (9.07%). Acute toxicity test was performed on hamsters and showed complete survival after 14 days, and there were no toxicity symptoms occurred. This study demonstrated that these essential oils seemed to be destitute of toxic effect which could compromise the medicinal use of these plants in folk medicine.

Keywords: analysis mass spectrometry, antibacterial activities, acute toxicity, chemical constitutes, gas chromatography, weight gain, Peganum harmala

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Authors: Fatima Zohra Ibn Majdoub Hassani, Ivan Lavandera, Joseph Kreit

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This study explored the effects of different organic solvents, temperature, and the amount of glycerol on the alcohol dehydrogenase (ADH)-catalysed stereoselective reduction of different ketones. These conversions were then analyzed by gas chromatography. It was found that when the amount of deep eutectic solvents (DES) increases, it can improve the stereoselectivity of the enzyme although reducing its ability to convert the substrate into the corresponding alcohol. Moreover, glycerol was found to have a strong stabilizing effect on the ADH from Ralstonia sp. (E. coli/ RasADH). In the case of organic solvents, it was observed that the best conversions into the alcohols were achieved with DMSO and hexane. It was also observed that temperature decreased the ability of the enzyme to convert the substrates into the products and also affected the selectivity. In addition to that, the recycling of DES up to three times gave good conversions and enantiomeric excess results and glycerol showed a positive effect in the stability of various ADHs. Using RasADH, a good conversion and enantiomeric excess into the S-alcohol were obtained. It was found that an enhancement of the temperature disabled the stabilizing effect of glycerol and decreased the stereoselectivity of the enzyme. However, for other ADHs a temperature increase had an opposite positive effect, especially with ADH-T from Thermoanaerobium sp. One of the objectives of this study was to see the effect of cofactors such as NAD(P) on the biocatlysis activities of ADHs.

Keywords: alcohol dehydrogenases, DES, gas chromatography, RasADH

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Authors: Renata Gerhardt, Detlev Belder

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Raman spectroscopy has attracted much attention as a structurally descriptive and label-free detection method. It is particularly suited for chemical analysis given as it is non-destructive and molecules can be identified via the fingerprint region of the spectra. In this work possibilities are investigated how to integrate Raman spectroscopy as a detection method for chip-based chromatography, making use of a droplet interface. A demanding task in lab-on-a-chip applications is the specific and sensitive detection of low concentrated analytes in small volumes. Fluorescence detection is frequently utilized but restricted to fluorescent molecules. Furthermore, no structural information is provided. Another often applied technique is mass spectrometry which enables the identification of molecules based on their mass to charge ratio. Additionally, the obtained fragmentation pattern gives insight into the chemical structure. However, it is only applicable as an end-of-the-line detection because analytes are destroyed during measurements. In contrast to mass spectrometry, Raman spectroscopy can be applied on-chip and substances can be processed further downstream after detection. A major drawback of Raman spectroscopy is the inherent weakness of the Raman signal, which is due to the small cross-sections associated with the scattering process. Enhancement techniques, such as surface enhanced Raman spectroscopy (SERS), are employed to overcome the poor sensitivity even allowing detection on a single molecule level. In SERS measurements, Raman signal intensity is improved by several orders of magnitude if the analyte is in close proximity to nanostructured metal surfaces or nanoparticles. The main gain of lab-on-a-chip technology is the building block-like ability to seamlessly integrate different functionalities, such as synthesis, separation, derivatization and detection on a single device. We intend to utilize this powerful toolbox to realize Raman detection in chip-based chromatography. By interfacing on-chip separations with a droplet generator, the separated analytes are encapsulated into numerous discrete containers. These droplets can then be injected with a silver nanoparticle solution and investigated via Raman spectroscopy. Droplet microfluidics is a sub-discipline of microfluidics which instead of a continuous flow operates with the segmented flow. Segmented flow is created by merging two immiscible phases (usually an aqueous phase and oil) thus forming small discrete volumes of one phase in the carrier phase. The study surveys different chip designs to realize coupling of chip-based chromatography with droplet microfluidics. With regards to maintaining a sufficient flow rate for chromatographic separation and ensuring stable eluent flow over the column different flow rates of eluent and oil phase are tested. Furthermore, the detection of analytes in droplets with surface enhanced Raman spectroscopy is examined. The compartmentalization of separated compounds preserves the analytical resolution since the continuous phase restricts dispersion between the droplets. The droplets are ideal vessels for the insertion of silver colloids thus making use of the surface enhancement effect and improving the sensitivity of the detection. The long-term goal of this work is the first realization of coupling chip based chromatography with droplets microfluidics to employ surface enhanced Raman spectroscopy as means of detection.

Keywords: chip-based separation, chip LC, droplets, Raman spectroscopy, SERS

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Authors: Sanja Podunavac-Kuzmanović, Strahinja Kovačević, Lidija Jevrić, Evgenija Djurendić, Jovana Ajduković

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There are several methods for determination of the lipophilicity of biologically active compounds, however chromatography has been shown as a very suitable method for this purpose. Chromatographic (C18-RP-HPLC) analysis of a series of 24 17-picolyl and 17-picolinylidene androstane derivatives was carried out. The obtained retention indices (logk, methanol (90%) / water (10%)) were correlated with calculated physicochemical and lipophilicity descriptors. The QSRR analysis was carried out applying principal component regression (PCR) and partial least squares regression (PLS). The PCR and PLS model were selected on the basis of the highest variance and the lowest root mean square error of cross-validation. The obtained PCR and PLS model successfully correlate the calculated molecular descriptors with logk parameter indicating the significance of the lipophilicity of compounds in chromatographic process. On the basis of the obtained results it can be concluded that the obtained logk parameters of the analyzed androstane derivatives can be considered as their chromatographic lipophilicity. These results are the part of the project No. 114-451-347/2015-02, financially supported by the Provincial Secretariat for Science and Technological Development of Vojvodina and CMST COST Action CM1105.

Keywords: androstane derivatives, chromatography, molecular structure, principal component regression, partial least squares regression

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Authors: Franz Zirena Vilca, Nestor Cahui Galarza, Walter Alejandro Zamalloa Cuba, Edith Tello Palma, Teofilo Donaires Flores, Valdemar Luiz Tornisielo

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The production of rainbow trout in the Lake Titicaca represents an important economic activity for Peru. The city of Puno is responsible for 83% of this production, so the use of antibiotics within the aquaculture system is not alien to this reality. Meanwhile, the waters of Lake Titicaca represent an important source for the supply of drinking water for 80% of the population of the Puno city. In this paper, twelve antibiotics for veterinary use were monitored in water samples during two seasons: dry (July 2015) and rainy (February 2016), water samples from trout production systems, near the water catching point in the lake and drinking water in the city house of Puno were considered. The samples were analyzed using liquid chromatography coupled to mass spectrometry and solid online phase extraction (On-line SPE-LC-MS/MS), all samples analyzed showed concentrations of Ciprofloxacin up to 65.2 ng L⁻¹ at the rainy season. On the other hand, 63% of water samples from the dry season and 36 % from the rainy season showed Chlortetracycline up to 8.7 and 6.1 ng L⁻¹, respectively. The presence of residues of veterinary antibiotics in drinking water means a serious health risk for 80% of the population of Puno since all these people are supplied from this source.

Keywords: chromatography, DNA damage, environmental risk, water pollution

Procedia PDF Downloads 193

Authors: I. Sarenkova, I. Ciprovica, I. Cinkmanis

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Lactobionic acid is a disaccharide formed from gluconic acid and galactose, and produced by oxidation of lactose. Productivity of lactobionic acid by microbial synthesis can be affected by various factors, and one of them is a presence of potassium, magnesium and manganese ions. In order to extend lactobionic acid production efficiency, it is necessary to increase the yield of lactobionic acid by optimising the fermentation conditions and available substrates for Pseudomonas taetrolens growth. The object of the research was to determinate the application of K₂HPO₄, MnSO₄, MgSO₄ × 7H₂O salts in different concentration for effective lactose oxidation to lactobionic acid by Pseudomonas taetrolens. Pseudomonas taetrolens NCIB 9396 (NCTC, England) and Pseudomonas taetrolens DSM 21104 (DSMZ, Germany) were used for the study. The acid whey was used as the study object. The content of lactose in whey samples was determined using MilcoScan^TM Mars (Foss, Denmark) and high performance liquid chromatography (Shimadzu LC 20 Prominence, Japan). The content of lactobionic acid in whey samples was determined using the high performance liquid chromatography. The impact of studied salts differs, Mn²⁺ and Mg²⁺ ions enhanced fermentation instead of K⁺ ions. Results approved that Mn²⁺ and Mg²⁺ ions are necessary for Pseudomonas taetrolens growth. The study results will help to improve the effectiveness of lactobionic acid production with Pseudomonas taetrolens NCIB 9396 and DSM 21104.

Keywords: lactobionic acid, lactose oxidation, Pseudomonas taetrolens, whey

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Authors: Dewi Selvia Fardhyanti, Astrilia Damayanti

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Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kind of useful compounds such as benzoic aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. The coal tar was collected by pyrolysis process of coal obtained from PT Kaltim Prima Coal and Arutmin-Kalimantan. The experiments typically occurred at the atmospheric pressure in a laboratory furnace at temperatures ranging from 300 to 550oC with a heating rate of 10oC/min and a holding time of 1 hour at the pyrolysis temperature. Nitrogen gas has been used to obtain the inert condition and to carry the gaseous pyrolysis products. The pyrolysis transformed organic materials into gaseous components, small quantities of liquid, and a solid residue (coke) containing fixed amount of carbon and ash. The composition of gas which is produced from the pyrolysis is carbon monoxide, hydrogen, methane, and other hydrocarbon compounds. The gas was condensed and the liquid containing oil/tar and water was obtained. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the coal tar components. The obtained coal tar has the viscosity of 3.12 cp, the density of 2.78 g/cm3, the calorific value of 11,048.44 cal/g, and the molecular weight of 222.67. The analysis result showed that the coal tar contained more than 78 chemical compounds such as benzene, cresol, phenol, xylene, naphtalene, etc. The total phenolic compounds contained in coal tar is 33.25% (PT KPC) and 17.58% (Arutmin-Kalimantan). The total naphtalene compounds contained in coal tar is 14.15% (PT KPC) and 17.13% (Arutmin-Kalimantan).

Keywords: coal tar, pyrolysis, gas chromatography-mass spectroscopy

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Authors: Tengku Muhammad Rafi Nazmi Bin Tengku Razali, Habsah Alwi

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This article based on effect of temperature towards extraction of Aquilaria Subintegra. Aquilaria Subintegra which its main habitat is in Asia-tropical and particularly often found in its native which is Thailand. There is claim which is Aquilaria Subintegra contains antipyretic properties that helps fight fever. Research nowadays also shown that paracetamol consumed bring bad effect towards consumers. This sample will first dry using Vacuum Far Infrared which provides better drying than conventional oven. Soxhlet extractor used to extract oil from sample. Gas Chromatography Mass Spectrometer used to analyze sample to determine its compound. Objective from this research was to determine the active ingredients that exist in the Aquilaria Subintegra leaves and to determine whether compound of Acetaminophen exist or not inside the leaves. Moisture content from 400C was 80%, 500C was 620% and 600C was 36%. The greater temperature resulting lower moisture content inside sample leaves. 7 components were identified in sample T=400C while only 5 components were identified in sample at T=50C and T=60C. Four components were commonly identified in three sample which is 1n-Hexadecanoic acid, 9,12,15-Octadecatrienoic acid, methyl ester (z,z,z), Vitamin E and Squalene. Further studies are needed with new series of temperature to refine the best results.

Keywords: aquilaria subintegra, vacuum far infrared, SOXHLET extractor, gas chromatography mass spectrometer, paracetamol

Procedia PDF Downloads 450

Authors: G. Dan Chépo, L. Ban-Koffi, N. Kouassi Kouakou, M. Dje Kouakou, J. Nemlin, A. Sahore Drogba, L. Kouame Patrice

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Solanum anguivi Lam, collectively called Gnagnan in Côte d'Ivoire is an eggplant with nutritional and therapeutic potentialities more or less known. The present study was undertaken to analyze the biochemical composition of berries at the different stages of maturity. Data showed that at the first stage of maturity (green berries), fruits are rich in ascorbic acid (34.48 ± 1.7 mg / 100 g dm), phenolic compounds (956.7 ± 71.14 mg / 100 g dm), iron (467.7 ± 1.84 mg / 100 g dm), magnesium (404.6 ± 16.25 mg / 100 g dm) and potassium (404.64 ± 16.25 mg/100 g dm). However, at the last stage of maturity (red berries), fruits are rich in proteins, cellulose, total sugars, fat and potassium with the values of 22.53 ± 2 g/100 g dm, 19.12 ± 0.35 g/100 g dm, 3.7 ± 0.2 g/100 g dm, 2.65 ± 0.19 g/100 g dm and 2290.84 ± 22.24 mg / 100 g dm, respectively. The chromatography on thin layer revealed the presence of glucose, ribose, xylose, arabinose and fructose at all the maturity stages. Except for alkaloids and gallic tannins, the phytochemical sorting revealed that Gnagnan contain many pharmacological components. According to the maturity stages, orange and red berries showed a higher content in sterols and polyterpens, flavonoids and saponins. The green berries contain most of polyphenols, catechintannins and quinons. As for the yellow berries, they are rich in polyphenols and catechintannins. These data contribute to enhance clinical researches on nutritional and pharmacological properties of S. anguivi Lam.

Keywords: Gnagnan, maturity stage, chemical composition, chromatography thin layer, phytochemical sorting

Procedia PDF Downloads 463