Search results for: liquid chromatography–mass spectrometry

Authors: Omasan Urhie Urhie, Adenipekun C. O, Eke W., Ogwu K., Erinle K. O

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Polychlorinated Biphenyls (PCBs) are Persistent organic pollutants (POPs) that are very toxic; they possess ability to accumulate in soil and in human tissues hence resulting in health issues like birth defect, reproductive disorder and cancer. The air is polluted by PCBs through volatilization and dispersion; they also contaminate soil and sediments and are not easily degraded. Soil samples were collected from a depth of 0-15 cm from three substations (Warri, Ughelli and Ibadan) of Power Holding Company of Nigeria (PHCN) where old transformers were dumped in Nigeria. Extraction and cleanup of soil samples were conducted using Accelerated Solvent Extraction (ASE) with Pressurized Liquid extraction (PLE). The concentration of PCBs was determined using gsas chromatography/mass spectrometry (GC/MS). Mean total PCB concentrations in the soil samples increased in the order Ughelli ˂ Ibadan˂ Warri, 2.457757ppm Ughelli substation 4.198926ppm, for Ibadan substation and 14.05065ppm at Warri substation. In the Warri samples, PCB-167 was the most abundant at about 30% (4.28086ppm) followed by PCB-157 at about 20% (2.77871), of the total PCB concentrations (14.05065ppm). Of the total PCBs in the Ughelli and Ibadan samples, PCB-156 was the most abundant at about 44% and 40%, respectively. This study provides a baseline report on the presence of PCBs in the vicinity of abandoned electrical power facilities in different cities in Nigeria.

Keywords: polychlorintated biphenyls, persistent organic pollutants, soil, transformer

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Authors: Anupalli Roja Rani, Pavithra Dasari

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Background: Among several, breast cancer has emerged as the most common female cancer in developing countries. It is the most common cause of cancer-related deaths worldwide among women. It is a molecularly and clinically heterogeneous disease. Moreover, it is a hormone–dependent tumor in which estrogens can regulate the growth of breast cells by binding with estrogen receptors (ERs). Moreover, the use of natural products in cancer therapeutics is due to their properties of biocompatibility and less toxicity. Plants are the vast reservoirs for various bioactive compounds. Coleus barbatus (Lamiaceae) contains anticancer properties against several cancer cell lines. Method: In the present study, an attempt is being made to enrich the knowledge of the anticancer activity of pure compounds extracted from Coleus barbatus (Andrew). On human breast cancer cell lines MCF-7. Here in, we are assessing the antiproliferative activity of Coleus barbatus (Andrew) plant extracts against MCF 7 and also evaluating their toxicity in normal human mammary cell lines such as Human Mammary Epithelial Cells (HMEC). The active fraction of plant extract was further purified with the help of Flash chromatography, Medium Pressure Liquid Chromatography (MPLC) and preparative High-Performance Liquid Chromatography (HPLC). The structure of pure compounds will be elucidated by using modern spectroscopic methods like Nuclear magnetic resonance (NMR), Electrospray Ionisation Mass Spectrometry (ESI-MS) methods. Later, the growth inhibition morphological assessment of cancer cells and cell cycle analysis of purified compounds were assessed using FACS. The growth and progression of signaling molecules HER2, GRP78 was studied by secretion assay using ELISA and expression analysis by flow cytometry. Result: Cytotoxic effect against MCF-7 with IC50 values were derived from dose response curves, using six concentrations of twofold serially diluted samples, by SOFTMax Pro software (Molecular device) and respectively Ellipticine and 0.5% DMSO were used as a positive and negative control. Conclusion: The present study shows the significance of various bioactive compounds extracted from Coleus barbatus (Andrew) root material. It acts as an anti-proliferative and shows cytotoxic effects on human breast cancer cell lines MCF7. The plant extracts play an important role pharmacologically. The whole plant has been used in traditional medicine for decades and the studies done have authenticated the practice. Earlier, as described, the plant has been used in the ayurveda and homeopathy medicine. However, more clinical and pathological studies must be conducted to investigate the unexploited potential of the plant. These studies will be very useful for drug designing in the future.

Keywords: coleus barbatus, HPLC, MPLC, NMR, MCF7, flash chromatograph, ESI-MS, FACS, ELISA.

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Authors: A. Durgadevi, S. Pushpavanam

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For the past several decades, CO2 levels have been dramatically increasing in the atmosphere due to the man-made emissions such as fossil fuel-fired power plants. With the increase in CO2 emissions, CO2 concentration in the atmosphere has increased resulting in global warming. This shows the need to study different ways to capture the emitted CO2 directly from the exhausts of power plants or atmosphere. There are several ways to remove CO2, such as absorption into a liquid solvent, adsorption into a solid, cryogenic separation, permeation through membranes and photochemical conversion. In most industries, the absorption of CO2 in chemical solvents (in absorption towers) is used for CO2 capture. In these towers, the mass transfer along with chemical reactions take place between the gas and liquid phase. This helps in the separation of CO2 from other gases. It is important to understand these processes in detail. These flow patterns are difficult to maintain in large scale industrial absorbers. So to get accurate information controlled gas-liquid absorption experiments are carried out in milli-channels in this work under controlled atmosphere. The absorption experiments of CO2 in varying concentrations of sodium hydroxide solution are carried out in T-junction glass milli-channels with a circular cross section (inner diameter of 2mm). The gas and liquid flow rates are controlled by a mass flow controller (MFC) and a Harvard syringe pump respectively. The slug flow in the channel is recorded using a camera and the videos are analysed. The gas slug of pure CO2 is found to decrease in size along the length of the channel due to absorption of gas in the liquid. This is also captured with the model developed and the mass transfer characteristics are studied. The pressure drop across the channel is determined by sum of the pressure drops from the gas slugs and the liquid plugs. A dimensionless correlation for the mass transfer coefficient is developed in terms of Sherwood number and compared with the existing correlations in the literature. They are found to be in close agreement with each other. In this case, due to the presence of chemical reaction, the enhancement of mass transfer is obtained. This is quantified with the help of an enhancement factor.

Keywords: absorption, enhancement factor, mass transfer coefficient, Sherwood number

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Authors: Malee Santikunaporn, Neera Wongtyanuwat, Channarong Asavatesanupap

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Pyrolysis of waste oil is an effective process to produce high quality liquid fuels. In this work, pyrolysis experiments of waste oil over Y zeolite were carried out in a semi-batch reactor under a flow of nitrogen at atmospheric pressure and at different reaction temperatures (350-450 ^oC). The products were gas, liquid fuel, and residue. Only liquid fuel was further characterized for its composition and properties by using gas chromatography, thermogravimetric analyzer, and bomb calorimeter. Experimental results indicated that the pyrolysis reaction temperature significantly affected both yield and composition distribution of pyrolysis oil. An increase in reaction temperature resulted in increased fuel yield, especially gasoline fraction. To obtain high amount of fuel, the optimal reaction temperature should be higher than 350 ^oC. A presence of Y zeolite in the system enhanced the cracking activity. In addition, the pyrolysis oil yield is proportional to the catalyst quantity.

Keywords: gasoline, diesel, pyrolysis, waste oil, Y zeolite

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Authors: Rabia Waseem, Low Kah Hin, Najihah Mohamed Hashim

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The variability in the chemical components of the Syzygium species essential oils has been evaluated. The leaves of Syzygium species have been collected from Perak, Malaysia. The essential oils extracted by using the conventional Hydro-distillation extraction procedure and analyzed by using Gas chromatography System attached with Mass Spectrometry (GCMS). Twenty-seven constituents were found in Syzygium species in which the major constituents include: α-Pinene (3.94%), α-Thujene (2.16%), α-Terpineol (2.95%), g-Elemene (2.89%) and D-Limonene (14.59%). The aim of this study was the comparison between the evaluated data and existing literature to fortify the major variability through statistical analysis.

Keywords: chemotaxonomy, cluster analysis, essential oil, medicinal plants, statistical analysis

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Authors: Meghana Shankara, Priyadarshini Natarajan

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Infrared (IR) spectroscopy has revolutionized the way we look at materials around us. Unraveling the pattern in the molecular spectra of materials to analyze the composition and properties of it has been one of the most interesting challenges in modern science. Applications of the IR spectrometry are numerous in the field’s pharmaceuticals, health, food and nutrition, oils, agriculture, construction, polymers, beverage, fabrics and much more limited only by the curiosity of the people. Near Infrared (NIR) spectrometry is applied robustly in analyzing the solids and liquid substances because of its non-destructive analysis method. In this paper, we have reviewed the application of NIR spectrometry in milk quality analysis and have presented the modes of measurement applied in NIRS measurement setup, Design of Experiment (DoE), classification/quantification algorithms used in the case of milk composition prediction like Fat%, Protein%, Lactose%, Solids Not Fat (SNF%) along with different approaches for adulterant identification. We have also discussed the important NIR ranges for the chosen milk parameters. The performance metrics used in the comparison of the various Chemometric approaches include Root Mean Square Error (RMSE), R^2, slope, offset, sensitivity, specificity and accuracy

Keywords: chemometrics, design of experiment, milk quality analysis, NIRS measurement modes

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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: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

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In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS

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Authors: Bernadett Henn, Katalin Tálos, Éva Kováss Széles

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During the last 50 years, the worldwide permeation of the nuclear techniques induces several new problems in the environmental and in the human life. Nowadays, due to the increasing of the risk of terrorism worldwide, the potential occurrence of terrorist attacks using also weapon of mass destruction containing radioactive or nuclear materials as e.g. dirty bombs, is a real threat. For instance, the uranium pellets are one of the potential nuclear materials which are suitable for making special weapons. The nuclear forensics mainly focuses on the determination of the origin of the confiscated or found nuclear and other radioactive materials, which could be used for making any radioactive dispersive device. One of the most important signatures in nuclear forensics to find the origin of the material is the determination of the rare earth element patterns (REE) in the seized or found radioactive or nuclear samples. The concentration and the normalized pattern of the REE can be used as an evidence of uranium origin. The REE are the fourteen Lanthanides in addition scandium and yttrium what are mostly found together and really low concentration in uranium pellets. The problems of the REE determination using ICP-MS technique are the uranium matrix (high concentration of uranium) and the interferences among Lanthanides. In this work, our aim was to develop an effective chemical sample preparation process using extraction chromatography for separation the uranium matrix and the rare earth elements from each other following some publications can be found in the literature and modified them. Secondly, our purpose was the optimization of the ICP-MS measuring process for REE concentration. During method development, in the first step, a REE model solution was used in two different types of extraction chromatographic resins (LN® and TRU®) and different acidic media for environmental testing the Lanthanides separation. Uranium matrix was added to the model solution and was proved in the same conditions. Methods were tested and validated using REE UOC (uranium ore concentrate) reference materials. Samples were analyzed by sector field mass spectrometer (ICP-SFMS).

Keywords: extraction chromatography, nuclear forensics, rare earth elements, uranium

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Authors: Bilal Murtaza, Xiaoyu Li, Liming Dong, Muhammad Kashif Saleemi, Gen Li, Bowen Jin, Lili Wang, Yongping Xu

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Fusarium spp. produce numerous mycotoxins, such as zearalenone (ZEN), deoxynivalenol (DON), and its acetylated compounds, 3-acetyl-deoxynivalenol (3-ADON) and 15-acetyl-deoxynivalenol (15-ADON) (15-ADON). In a co-culture system, the soil-derived Escherichia marmotae strain degrades ZEN and DON into 3-keto-DON and DOM-1 via enzymatic deep-oxidation. When pure mycotoxins were subjected to Escherichia marmotae in culture flasks, degradation, and detoxification were also attained. DON and ZEN concentrations, ambient pH, incubation temperatures, bacterium concentrations, and the impact of acid treatment on degradation were all evaluated. The results of the ELISA and high-performance liquid chromatography-electrospray ionization-high resolution mass spectrometry (HPLC-ESI-HRMS) tests demonstrated that the concentration of mycotoxins exposed to Escherichia marmotae was significantly lower than the control. ZEN levels were reduced by 43.9%, while zearalenone sulfate ([M/z 397.1052 C18H21O8S1) was discovered as a derivative of ZEN converted by microbes to a less toxic molecule. Furthermore, Escherichia marmotae appeared to metabolize DON 35.10% into less toxic derivatives (DOM-1 at m/z 281 of [DON - O]+ and 3-keto-DON at m/z 295 of [DON - 2H]+). These results show that Escherichia marmotae can reduce Fusarium mycotoxins production, degrade pure mycotoxins, and convert them to less harmful compounds, opening up new possibilities for study and innovation in mycotoxin detoxification.

Keywords: mycotoxins, zearalenone, deoxynivalenol, bacterial degradation

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Authors: Serkan Sayin, Songul F. Varol

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High attention on the organic light-emitting diodes has been paid since their efficient properties in the flat panel displays, and solid-state lighting was realized. Because of their high efficient electroluminescence, brightness and providing eminent in the emission range, organic light emitting diodes have been preferred a material compared with the other materials consisting of the liquid crystal. Calixarenes obtained from the reaction of p-tert-butyl phenol and formaldehyde in a suitable base have been potentially used in various research area such as catalysis, enzyme immobilization, and applications, ion carrier, sensors, nanoscience, etc. In addition, their tremendous frameworks, as well as their easily functionalization, make them an effective candidate in the applied chemistry. Herein, a calix[4]arene derivative has been synthesized, and its structure has been fully characterized using Fourier Transform Infrared Spectrophotometer (FTIR), proton nuclear magnetic resonance (¹H-NMR), carbon-13 nuclear magnetic resonance (¹³C-NMR), liquid chromatography-mass spectrometry (LC-MS), and elemental analysis techniques. The calixarene derivative has been employed as an emitting layer in the fabrication of the organic light-emitting diodes. The optical and electrochemical features of calixarane-contained organic light-emitting diodes (Clx-OLED) have been also performed. The results showed that Clx-OLED exhibited blue emission and high external quantum efficacy. As a conclusion obtained results attributed that the synthesized calixarane derivative is a promising chromophore with efficient fluorescent quantum yield that provides it an attractive candidate for fabricating effective materials for fluorescent probes and labeling studies. This study was financially supported by the Scientific and Technological Research Council of Turkey (TUBITAK Grant no. 117Z402).

Keywords: calixarene, OLED, supramolecular chemistry, synthesis

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Authors: H. Troudi, M. Ghiss, Z. Tourki, M. Ellejmi

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Packed columns of liquefied petroleum gas (LPG) consists of separating the liquid mixture of propane and butane to pure gas components by the distillation phenomenon. The flow of the gas and liquid inside the columns is operated by two ways: The co-current and the counter current operation. Heat, mass and species transfer between phases represent the most important factors that influence the choice between those two operations. In this paper, both processes are discussed using computational CFD simulation through ANSYS-Fluent software. Only 3D half section of the packed column was considered with one packed bed. The packed bed was characterized in our case as a porous media. The simulations were carried out at transient state conditions. A multi-component gas and liquid mixture were used out in the two processes. We utilized the Euler-Lagrange approach in which the gas was treated as a continuum phase and the liquid as a group of dispersed particles. The heat and the mass transfer process was modeled using multi-component droplet evaporation approach. The results show that the counter-current process performs better than the co-current, although such limitations of our approach are noted. This comparison gives accurate results for computations times higher than 2 s, at different gas velocity and at packed bed porosity of 0.9.

Keywords: co-current, counter-current, Euler-Lagrange model, heat transfer, mass transfer

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Authors: Marcela dos P. G. Baltazar, Louise H. Gracioso, Luciana J. Gimenes, Bruno Karolski, Ingrid Avanzi, Elen A. Perpetuo

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In this work, bacterial strains were isolated from environmental samples from a copper mine and three of them presented potential for bioremediation of copper. All the strains were identified by mass spectrometry (MALDI-TOF-Biotyper) and grown in three diferent media supplemented with 100 ppm of copper chloride in flasks of 500mL and it was incubated at 28 °C and 180 rpm. Periodically, samples were taken and monitored for cellular growth and copper biosorption by spectrophotometer UV-Vis (600 nm) and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), respectively. At the end of exponential phase of cellular growth, the biomass was utilized to construct a correlation curve between absorbance and dry mass of the cells. Among the three isolates with potential for biorremediation, 1 strain exhibit capacity the most for bioremediation of effluents contaminated by copper being identified as Rhodococcus erythropolis.

Keywords: bioprocess, bioremediation, biosorption, copper

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Authors: Yen-An Tsai, Ching-Ling Lin, Jia-Woei Hou, Mei-Lien Chen

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Endocrine-disrupting chemicals (EDCs) adversely affect the endocrine system. Phthalates, also called phthalic acid esters (PAEs), are manmade chemicals that are used as stabilizing agents in personal care products such as perfumes, lotions, and cosmetics. The aim was to explore whether PAEs exposure was associated with central precocious puberty (CPP) or constitutional delays in growth (CDGP). This case-control study included 48 female with CPP, 37 male with constitutional delays in growth, and 127 normal children and was conducted from December 2011 to August 2014. All participants completed a structured questionnaire regarding socio-demographic characteristics, lifestyle, and secondary sexual characteristics. The analytical method was based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with isotope dilution for the quantitative detection of several phthalate metabolites in human urine. The risk of CPP with mep, mnbp, LMW >50th percentile were higher than those with 50th percentile were higher than those with <50 percentile in model 2. In model 1, we only found higher CDGP risk in mep, mnbp, and ΣPAEs. It shows that high phthalate exposure may associate with CDGP. In this case-control study, we found PAEs exposure was associated with central precocious puberty (CPP) or constitutional delays in growth.

Keywords: phthalates, puberty, delays, growth

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Authors: Mohammed Falalu Hamza

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A phytochemical investigation conducted on the leaves extract of Cryptocarya latifolia (Lauraceae) revealed the presence of two major essential oils; Nerolidol (1) and Copaene (2) with the aid of gas chromatography-mass spectrometry (GC-MS). The compounds exhibited good anti-oxidant capacity using 2,2-diphenyl-1-picryl-hydrazyl (DPPH) radical scavenging assay. The result shows that the anti-oxidant capacity of the compounds is dependent on concentration similar to the standard (ascorbic acid). This study shows that the leaves extract of C. latifolia is a good source of important natural antioxidants.

Keywords: broad-leaved quince, phytochemical, anti-oxidant, essential oils

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Authors: Anjana Sagar

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Arsenic poisoned ground water is a major concern in South Asia. The arsenic enters the food chain not only through drinking but also by using arsenic polluted water for irrigation. Arsenic is highly toxic in its inorganic forms; however, organic forms of arsenic are comparatively less toxic. In terrestrial plants, inorganic form of arsenic is predominantly found; however, we found that significant proportion of organic arsenic was present in root and shoot of a staple legume, chickpea (Cicer arientinum L) plants. Chickpea plants were raised in pot culture on soils spiked with arsenic ranging from 0-70 mg arsenate per Kg soil. Total arsenic concentrations of chickpea shoots and roots were determined by inductively coupled plasma-mass-spectrometry (ICP-MS) ranging from 0.76 to 20.26, and 2.09 to 16.43 µg g⁻¹ dry weight, respectively. Information on arsenic species was acquired by methanol/water extraction method, with arsenic species being analyzed by high-performance liquid chromatography (HPLC) coupled with ICP-MS. Dimethylarsinic acid (DMA) was the only organic arsenic species found in amount from 0.02 to 3.16 % of total arsenic shoot concentration and 0 to 6.93 % of total arsenic root concentration, respectively. To investigate the source of the organic arsenic in chickpea plants, arsenic species in the rhizosphere of soils of plants were also examined. The absence of organic arsenic in soils would suggest the possibility of formation of DMA in plants. The present investigation provides useful information for better understanding of distribution of arsenic species in terrestrial legume plants.

Keywords: arsenic, arsenic speciation, dimethylarsinic acid, organoarsenic

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Authors: Silvia Portarena, Chiara Anselmi, Chiara Baldacchini, Enrico Brugnoli

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Extra virgin olive oil (EVOO) is a complex matrix mainly composed by fatty acid and other minor compounds, among which carotenoids are well known for their antioxidative function that is a key mechanism of protection against cancer, cardiovascular diseases, and macular degeneration in humans. EVOO composition in terms of such constituents is generally the result of a complex combination of genetic, agronomical and environmental factors. To selectively improve the quality of EVOOs, the role of each factor on its biochemical composition need to be investigated. By selecting fruits from four different cultivars similarly grown and harvested, it was demonstrated that Raman spectroscopy, combined with chemometric analysis, is able to discriminate the different cultivars, also as a function of the harvest date, based on the relative content and composition of fatty acid and carotenoids. In particular, a correct classification up to 94.4% of samples, according to the cultivar and the maturation stage, was obtained. Moreover, by using gas chromatography and high-performance liquid chromatography as reference techniques, the Raman spectral features further allowed to build models, based on partial least squares regression, that were able to predict the relative amount of the main fatty acids and the main carotenoids in EVOO, with high coefficients of determination. Besides genetic factors, climatic parameters, such as light exposition, distance from the sea, temperature, and amount of precipitations could have a strong influence on EVOO composition of both major and minor compounds. This suggests that the Raman spectra could act as a specific fingerprint for the geographical discrimination and authentication of EVOO. To understand the influence of environment on EVOO Raman spectra, samples from seven regions along the Italian coasts were selected and analyzed. In particular, it was used a dual approach combining Raman spectroscopy and isotope ratio mass spectrometry (IRMS) with principal component and linear discriminant analysis. A correct classification of 82% EVOO based on their regional geographical origin was obtained. Raman spectra were obtained by Super Labram spectrometer equipped with an Argon laser (514.5 nm wavelenght). Analyses of stable isotope content ratio were performed using an isotope ratio mass spectrometer connected to an elemental analyzer and to a pyrolysis system. These studies demonstrate that RR spectroscopy is a valuable and useful technique for the analysis of EVOO. In combination with statistical analysis, it makes possible the assessment of specific samples’ content and allows for classifying oils according to their geographical and varietal origin.

Keywords: authentication, chemometrics, olive oil, raman spectroscopy

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Authors: Anil P. Dewani, Alok S. Tripathi, Anil V. Chandewar

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Present manuscript reports the development and validation of a quantitative high performance liquid chromatography method for the pharmacokinetic evaluation of Glimepiride (GLM) and Ilaprazole (ILA) in rat plasma. The plasma samples were involved with Solid phase extraction process (SPE). The analytes were resolved on a Phenomenex C18 column (4.6 mm× 250 mm; 5 µm particle size) using a isocratic elution mode comprising methanol:water (80:20 % v/v) with pH of water modified to 3 using Formic acid, the total run time was 10 min at 225 nm as common wavelength, the flow rate throughout was 1ml/min. The method was validated over the concentration range from 10 to 600 ng/mL for GLM and ILA, in rat plasma. Metformin (MET) was used as Internal Standard. Validation data demonstrated the method to be selective, sensitive, accurate and precise. The limit of detection was 1.54 and 4.08 and limit of quantification was 5.15 and 13.62 for GLM and ILA respectively, the method demonstrated excellent linearity with correlation coefficients (r2) 0.999. The intra and inter-day precision (RSD%) values were < 2.0% for both ILA and GLM. The method was successfully applied in pharmacokinetic studies followed by oral administration in rats.

Keywords: pharmacokinetics, glimepiride, ilaprazole, HPLC, SPE

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Authors: Yuting Wu, Faraz Choudhury, Daniel Benjamin, James Whalin, Joshua Blatz, Leon Shohet, Michael Sussman, Mark Richards

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Plasma-Induced Modification of Biomolecules (PLIMB) has been developed as a technology, which, together with mass spectrometry, measures three-dimensional structural characteristics of proteins. This technique uses hydroxyl radicals generated by atmospheric-pressure plasma discharge to react with the solvent-accessible side chains of protein in an aqueous solution. In this work, we investigate the three-dimensional structure of hemoglobin and myoglobin using PLIMB. Additional modifications to these proteins, such as oxidation, fragmentations, and conformational changes caused by PLIMB are also explored. These results show that PLIMB, coupled with mass spectrometry, is an effective way to determine solvent access to hemoproteins. Furthermore, we show that many factors, including pH and the electrical parameters used to generate the plasma, have a significant influence on solvent accessibility.

Keywords: plasma, hemoglobin, myoglobin, solvent access

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Authors: Huixia Shi, Can Hu, Jun Zhu, Hongling Guo, Haiyan Li, Hongyan Du

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The identification of human body fluids during forensic investigations is a critical step to determine key details, and present strong evidence to testify criminal in a case. With the popularity of DNA and improved detection technology, the potential question must be revolved that whether the suspect’s DNA derived from saliva or semen, menstrual or peripheral blood, how to identify the red substance or aged blood traces on the spot is blood; How to determine who contribute the right one in mixed stains. In recent years, molecular approaches have been developing increasingly on mRNA, miRNA, DNA methylation and microbial markers, but appear expensive, time-consuming, and destructive disadvantages. Physicochemical methods are utilized frequently such us scanning electron microscopy/energy spectroscopy and X-ray fluorescence and so on, but results only showing one or two characteristics of body fluid itself and that out of working in unknown or mixed body fluid stains. This paper focuses on using chemistry methods Raman spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry to discriminate species of peripheral blood, menstrual blood, semen, saliva, vaginal secretions, urine or sweat. Firstly, non-destructive, confirmatory, convenient and fast Raman spectroscopy method combined with more accurate matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method can totally distinguish one from other body fluids. Secondly, 11 spectral signatures and specific metabolic molecules have been obtained by analysis results after 70 samples detected. Thirdly, Raman results showed peripheral and menstrual blood, saliva and vaginal have highly similar spectroscopic features. Advanced statistical analysis of the multiple Raman spectra must be requested to classify one to another. On the other hand, it seems that the lactic acid can differentiate peripheral and menstrual blood detected by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, but that is not a specific metabolic molecule, more sensitivity ones will be analyzed in a forward study. These results demonstrate the great potential of the developed chemistry methods for forensic applications, although more work is needed for method validation.

Keywords: body fluids, identification, Raman spectroscopy, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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Authors: Abid Fida Masih

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Forced degradation study of Rifaximin was conducted to determine the stability indicating potential of HPLC testing method for detection of Rifaximin in formulated tablets to be employed for quality control and stability testing. The questioned method applied with mobile phase methanol: water (70:30), 5µm, 250 x 4.6mm, C18 column, wavelength 293nm and flow rate of 1.0 ml/min. Forced degradation study was performed under oxidative, acidic, basic, thermal and photolytic conditions. The applied method successfully determined the degradation products after acidic and basic degradation without interfering with Rifaximin detection. Therefore, the method was said to be stability indicating and can be applied for quality control and stability testing of Rifaxmin tablets during its shelf life.

Keywords: forced degradation, high-performance liquid chromatography, method validation, rifaximin, stability indicating method

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Authors: Harshani Uggallage, Kapila D. Dissanayaka

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A Sulforhodamine-B assay-guided fractionation on Nigella sativa seeds was conducted to determine the presence of cytotoxic compounds against human hepatoma (HepG2) cells. Initially, a freeze-dried sample of Nigella sativa seeds was sequentially extracted into solvents of increasing polarities. Crude extracts from the sequential extraction of Nigella sativa seeds in chloroform and ethyl acetate showed the highest cytotoxicity. The combined mixture of these two extracts was subjected to bioassay guided fractionation using a modified Kupchan method of partitioning, followed by Sephadex® LH-20 chromatography. This chromatographic separation process resulted in a column fraction with a convincing IC50 (half-maximal inhibitory concentration) value of 13.07µg/ml, which is considerable for developing therapeutic drug leads against human hepatoma. Reversed phase High-Performance Liquid Chromatography (HPLC) was finally conducted for the same column fraction, and the result indicates the presence of one or several main cytotoxic compounds against human HepG2 cells.

Keywords: cytotoxic compounds, half-maximal inhibitory concentration, high-performance liquid chromatography, human HepG2 cells, nigella sativa seeds, Sulforhodamine-B assay

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Authors: Ali M. EL-Soll

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Physical properties of Sarir waxy crude oil was investigated, pour-point was determined using ASTM D-79 procedure, paraffin content and carbon number distribution of the paraffin was determined using gas liquid Chromatography(GLC), polymeric additives were prepared and their structures were confirmed using IR spectrophotometer. The molecular weight and molecular weigh distribution of these additives were determined by gel permeation chromatography (GPC). the performance of the synthesized additives as pour-point depressants was evaluated, for the mentioned crude oil.

Keywords: sarir, waxy, crude, pour point, depressants

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Authors: Patricia O. Carvalho, Marcia C. F. Messias, Salvador Sanchez Vinces, Caroline F. A. Gatinoni, Vitor P. Iordanu, Carlos A. R. Martinez

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Lipidomics methods are widely used in the identification and validation of disease-specific biomarkers and therapy response evaluation. The present study aimed to identify a panel of potential lipid biomarkers to evaluate response to neoadjuvant chemoradiotherapy in rectal adenocarcinoma (RAC). Liquid chromatography–mass spectrometry (LC-MS)-based untargeted lipidomic was used to profile human serum samples from patients with clinical stage T2 or T3 resectable RAC, after and before chemoradiotherapy treatment. A total of 28 blood plasma samples were collected from 14 patients with RAC who recruited at the São Francisco University Hospital (HUSF/USF). The study was approved by the ethics committee (CAAE 14958819.8.0000.5514). Univariate and multivariate statistical analyses were applied to explore dysregulated metabolic pathways using untargeted lipidic profiling and data mining approaches. A total of 36 statistically significant altered lipids were identified and the subsequent partial least-squares discriminant analysis model was both cross validated (R2, Q2) and permutated. Lisophosphatidyl-choline (LPC) plasmalogens containing palmitoleic and oleic acids, with high variable importance in projection score, showed a tendency to be lower after completion of chemoradiotherapy. Chemoradiotherapy seems to change plasmanyl-phospholipids levels, indicating that these lipids play an important role in the RAC pathogenesis.

Keywords: lipidomics, neoadjuvant chemoradiotherapy, plasmalogens, rectal adenocarcinoma

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Authors: Itti Bist, Snehasis Bhakta, Di Jiang, Tia E. Keyes, Aaron Martin, Robert J. Forster, James F. Rusling

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DNA damage from metabolites of lipophilic drugs and pollutants, generated by enzymes, represents a major toxicity pathway in humans. These metabolites can react with DNA to form either 8-oxo-7,8-dihydro-2-deoxyguanosine (8-oxodG), which is the oxidative product of DNA or covalent DNA adducts, both of which are genotoxic and hence considered important biomarkers to detect cancer in humans. Therefore, detecting reactions of metabolites with DNA is an effective approach for the safety assessment of new chemicals and drugs. Here we describe a novel electrochemiluminescent (ECL) sensor array which can detect DNA oxidation and chemical DNA damage in a single array, facilitating a more accurate diagnostic tool for genotoxicity screening. Layer-by-layer assembly of DNA and enzyme are assembled on the pyrolytic graphite array which is housed in a microfluidic device for sequential detection of two type of the DNA damages. Multiple enzyme reactions are run on test compounds using the array, generating toxic metabolites in situ. These metabolites react with DNA in the films to cause DNA oxidation and chemical DNA damage which are detected by ECL generating osmium compound and ruthenium polymer, respectively. The method is further validated by the formation of 8-oxodG and DNA adduct using similar films of DNA/enzyme on magnetic bead biocolloid reactors, hydrolyzing the DNA, and analyzing by liquid chromatography-mass spectrometry (LC-MS). Hence, this combined DNA/enzyme array/LC-MS approach can efficiently explore metabolic genotoxic pathways for drugs and environmental chemicals.

Keywords: biosensor, electrochemiluminescence, DNA damage, microfluidic array

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Authors: Igor Jerkovic

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Biodiversity of flora provides many different nectar sources for the bees. Unifloral honeys possess distinctive flavours, mainly derived from their nectar sources (characteristic volatile organic components (VOCs)). Specific or nonspecific VOCs (chemical markers) could be used for unifloral honey characterisation as addition to the melissopalynologycal analysis. The main honey volatiles belong, in general, to three principal categories: terpenes, norisoprenoids, and benzene derivatives. Some of these substances have been described as characteristics of the floral source, and other compounds, like several alcohols, branched aldehydes, and furan derivatives, may be related to the microbial purity of honey processing and storage conditions. Selection of the extraction method for the honey volatiles profiling should consider that heating of the honey produce different artefacts and therefore conventional methods of VOCs isolation (such as hydrodistillation) cannot be applied for the honey. Two-way approach for the isolation of the honey VOCs was applied using headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE). The extracts were analysed by gas chromatography and mass spectrometry (GC-MS). HS-SPME (with the fibers of different polarity such as polydimethylsiloxane/ divinylbenzene (PDMS/DVB) or divinylbenzene/carboxene/ polydimethylsiloxane (DVB/CAR/PDMS)) enabled isolation of high volatile headspace VOCs of the honey samples. Among them, some characteristic or specific compounds can be found such as 3,4-dihydro-3-oxoedulan (in Centaurea cyanus L. honey) or 1H-indole, methyl anthranilate, and cis-jasmone (in Citrus unshiu Marc. honey). USE with different solvents (mainly dichloromethane or the mixture pentane : diethyl ether 1 : 2 v/v) enabled isolation of less volatile and semi-volatile VOCs of the honey samples. Characteristic compounds from C. unshiu honey extracts were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. Sometimes, the selection of solvent sequence was useful for more complete profiling such as sequence I: pentane → diethyl ether or sequence II: pentane → pentane/diethyl ether (1:2, v/v) → dichloromethane). The extracts with diethyl ether contained hydroquinone and 4-hydroxybenzoic acid as the major compounds, while (E)-4-(r-1’,t-2’,c-4’-trihydroxy-2’,6’,6’-trimethylcyclo-hexyl)but-3-en-2-one predominated in dichloromethane extracts of Allium ursinum L. honey. With this two-way approach, it was possible to obtain a more detailed insight into the honey volatile and semi-volatile compounds and to minimize the risks of compound discrimination due to their partial extraction that is of significant importance for the complete honey profiling and identification of the chemical biomarkers that can complement the pollen analysis.

Keywords: honey chemical biomarkers, honey volatile compounds profiling, headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE)

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Authors: Reyna Singh, David Lokhat, Milan Carsky

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The world crude oil demand is projected to rise to 108.5 million bbl/d by the year 2035. With reserves estimated at 869 billion tonnes worldwide, coal is an abundant resource. This work was aimed at producing a high value hydrocarbon liquid product from the Direct Coal Liquefaction (DCL) process at, comparatively, mild operating conditions. Via hydrogenation, the temperature-staged approach was investigated. In a two reactor lab-scale pilot plant facility, the objectives included maximising thermal dissolution of the coal in the presence of a hydrogen donor solvent in the first stage, subsequently promoting hydrogen saturation and hydrodesulphurization (HDS) performance in the second. The feed slurry consisted of high grade, pulverized bituminous coal on a moisture-free basis with a size fraction of < 100μm; and Tetralin mixed in 2:1 and 3:1 solvent/coal ratios. Magnetite (Fe3O4) at 0.25wt% of the dry coal feed was added for the catalysed runs. For both stages, hydrogen gas was used to maintain a system pressure of 100barg. In the first stage, temperatures of 250℃ and 300℃, reaction times of 30 and 60 minutes were investigated in an agitated batch reactor. The first stage liquid product was pumped into the second stage vertical reactor, which was designed to counter-currently contact the hydrogen rich gas stream and incoming liquid flow in the fixed catalyst bed. Two commercial hydrotreating catalysts; Cobalt-Molybdenum (CoMo) and Nickel-Molybdenum (NiMo); were compared in terms of their conversion, selectivity and HDS performance at temperatures 50℃ higher than the respective first stage tests. The catalysts were activated at 300°C with a hydrogen flowrate of approximately 10 ml/min prior to the testing. A gas-liquid separator at the outlet of the reactor ensured that the gas was exhausted to the online VARIOplus gas analyser. The liquid was collected and sampled for analysis using Gas Chromatography-Mass Spectrometry (GC-MS). Internal standard quantification methods for the sulphur content, the BTX (benzene, toluene, and xylene) and alkene quality; alkanes and polycyclic aromatic hydrocarbon (PAH) compounds in the liquid products were guided by ASTM standards of practice for hydrocarbon analysis. In the first stage, using a 2:1 solvent/coal ratio, an increased coal to liquid conversion was favoured by a lower operating temperature of 250℃, 60 minutes and a system catalysed by magnetite. Tetralin functioned effectively as the hydrogen donor solvent. A 3:1 ratio favoured increased concentrations of the long chain alkanes undecane and dodecane, unsaturated alkenes octene and nonene and PAH compounds such as indene. The second stage product distribution showed an increase in the BTX quality of the liquid product, branched chain alkanes and a reduction in the sulphur concentration. As an HDS performer and selectivity to the production of long and branched chain alkanes, NiMo performed better than CoMo. CoMo is selective to a higher concentration of cyclohexane. For 16 days on stream each, NiMo had a higher activity than CoMo. The potential to cover the demand for low–sulphur, crude diesel and solvents from the production of high value hydrocarbon liquid in the said process, is thus demonstrated.

Keywords: catalyst, coal, liquefaction, temperature-staged

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Authors: Rowan Moore, Kai Scheffler, Eugen Damoc, Jennifer Sutton, Aaron Bailey, Stephane Houel, Simon Cubbon, Jonathan Josephs

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Purpose: MS analysis of monoclonal antibodies (mAbs) at the protein and peptide levels is critical during development and production of biopharmaceuticals. The compositions of current generation therapeutic proteins are often complex due to various modifications which may affect efficacy. Intact proteins analyzed by MS are detected in higher charge states that also provide more complexity in mass spectra. Protein analysis in native or native-like conditions with zero or minimal organic solvent and neutral or weakly acidic pH decreases charge state value resulting in mAb detection at higher m/z ranges with more spatial resolution. Methods: Three commercially available mAbs were used for all experiments. Intact proteins were desalted online using size exclusion chromatography (SEC) or reversed phase chromatography coupled on-line with a mass spectrometer. For streamlined use of the LC- MS platform we used a single SEC column and alternately selected specific mobile phases to perform separations in either denaturing or native-like conditions: buffer A (20 % ACN, 0.1 % FA) with Buffer B (100 mM ammonium acetate). For peptide analysis mAbs were proteolytically digested with and without prior reduction and alkylation. The mass spectrometer used for all experiments was a commercially available Thermo Scientific™ hybrid Quadrupole-Orbitrap™ mass spectrometer, equipped with the new BioPharma option which includes a new High Mass Range (HMR) mode that allows for improved high mass transmission and mass detection up to 8000 m/z. Results: We have analyzed the profiles of three mAbs under reducing and native conditions by direct infusion with offline desalting and with on-line desalting via size exclusion and reversed phase type columns. The presence of high salt under denaturing conditions was found to influence the observed charge state envelope and impact mass accuracy after spectral deconvolution. The significantly lower charge states observed under native conditions improves the spatial resolution of protein signals and has significant benefits for the analysis of antibody mixtures, e.g. lysine variants, degradants or sequence variants. This type of analysis requires the detection of masses beyond the standard mass range ranging up to 6000 m/z requiring the extended capabilities available in the new HMR mode. We have compared each antibody sample that was analyzed individually with mixtures in various relative concentrations. For this type of analysis, we observed that apparent native structures persist and ESI is benefited by the addition of low amounts of acetonitrile and formic acid in combination with the ammonium acetate-buffered mobile phase. For analyses on the peptide level we analyzed reduced/alkylated, and non-reduced proteolytic digests of the individual antibodies separated via reversed phase chromatography aiming to retrieve as much information as possible regarding sequence coverage, disulfide bridges, post-translational modifications such as various glycans, sequence variants, and their relative quantification. All data acquired were submitted to a single software package for analysis aiming to obtain a complete picture of the molecules analyzed. Here we demonstrate the capabilities of the mass spectrometer to fully characterize homogeneous and heterogeneous therapeutic proteins on one single platform. Conclusion: Full characterization of heterogeneous intact protein mixtures by improved mass separation on a quadrupole-Orbitrap™ mass spectrometer with extended capabilities has been demonstrated.

Keywords: disulfide bond analysis, intact analysis, native analysis, mass spectrometry, monoclonal antibodies, peptide mapping, post-translational modifications, sequence variants, size exclusion chromatography, therapeutic protein analysis, UHPLC

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Authors: G. V. Manzane, S. J. Modise

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Uterine fibroids, also known as leiomyomas or myomas, are non-cancerous growths that develop in the muscular wall of the uterus during the reproductive years. The cause of uterine fibroids includes hormonal, genetic, growth factors, and extracellular matrix factors. Common symptoms of uterine fibroids include heavy and prolonged menstrual bleeding which can lead to a high risk of anemia, lower abdominal pains, pelvic pressure, infertility, and pregnancy loss. The growth of this tumor is a concern because of its negative impact on women’s health and the increase in their economic burden. Traditional medicinal plants have long been used in Africa for their potential therapeutic effects against various ailments. In this study, we aimed to identify and characterize bioactive compounds from selected African medicinal plants with potential anti-fibrotic properties using Fourier-transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometry (GCMS) analysis. Two medicinal plant species known for their traditional use in fibrosis-related conditions were selected for investigation. Aqueous extracts were prepared from the plant materials, and FTIR analysis was conducted to determine the functional groups present in the extracts. GCMS analysis was performed to identify the chemical constituents of the extracts. The FTIR analysis revealed the presence of various functional groups, such as phenols, flavonoids, terpenoids, and alkaloids, known for their potential therapeutic activities. These functional groups are associated with antioxidant, anti-inflammatory, and anti-fibrotic properties. The GCMS analysis identified several bioactive compounds, including flavonoids, alkaloids, terpenoids, and phenolic compounds, which are known for their pharmacological activities. The discovery of bioactive compounds in African medicinal plants that exhibit anti-fibrotic effects, opens up promising avenues for further research and development of potential treatments for fibrosis. This suggests the potential of these plants as a valuable source of novel therapeutic agents for treating fibrosis-related conditions. In conclusion, our study identified and characterized bioactive compounds from selected African medicinal plants using FTIR and GCMS analysis. The presence of compounds with known antifibrotic properties suggests that these plants hold promise as a potential source of natural products for the development of novel anti-fibrotic therapies.

Keywords: uterine fibroids, african medicinal plants, bioactive compounds, identify and characterized

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