Search results for: Gas Chromatography- Mass Spectrometry (GC-MS)

Authors: B. Y. Matmuratov, S. D. Madrakhimova. R. S. Esanov. A. D. Matchanov

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Supramolecular complexes of glycyrrhizic acid with kinetin in various molar ratios were obtained, physico-chemical parameters and spectral properties of the resulting complexes were studied (UV, IR, mass spectrometry.

Keywords: Monoammonium salt of glycyrrhizic acid, glycyrrhizic acid, supramolecular complex, isomolar series, IR spectroscopy.

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Authors: K. Jarmkom, P. Eakwaropas, W. Khobjai, S. Techaeoi

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Ancient Thai perfumed powder was used as a fragrance for clothing, food, and the body. Plant-based natural Thai perfume products are known as Pang-Rum. The objective of this study was to evaluate the stability of essential oils after six months of incubation. The chemical compositions were determined by gas chromatography-mass spectrometry (GC-MS), in terms of the qualitative composition of the isolated essential oil. The isolation of the essential oil of natural products by incubate sample for 5 min at 40 ºC is described. The volatile components were identified by percentage of total peak areas comparing their retention times of GC chromatograph with NIST mass spectral library. The results show no significant difference in the seven chromatograms of perfumed powder (Pang-Rum) both with binder and without binder. Further identification was done by GC-MS. Some components of Pang-Rum with/without binder were changed by temperature and time.

Keywords: GC-MS analysis, essential oils, stability, Pang-Rum.

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Authors: C. I. L. Justino, L. I. B. Silva, K. Duarte, A. C. Freitas, T. A. P. Rocha-Santos, A. C. Duarte

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This work proposes an optical fiber system (OF) for sensing various volatile organic compounds (VOCs) in human breath for the diagnosis of some metabolic disorders as a non-invasive methodology. The analyzed VOCs are alkanes (i.e., ethane, pentane, heptane, octane, and decane), and aromatic compounds (i.e., benzene, toluene, and styrene). The OF displays high analytical performance since it provides near real-time responses, rapid analysis, and low instrumentation costs, as well as it exhibits useful linear range and detection limits; the developed OF sensor is also comparable to a reference methodology (gas chromatography-mass spectrometry) for the eight tested VOCs.

Keywords: Breath analysis, gas chromatography-mass spectrometry, optical fiber sensor, volatile organic compounds

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Authors: M. Bounechada, F. Benia, M. Aiouaz, S. Bouharati, N. Djirar, H. Benamrani

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The cuticular hydrocarbons of Pamphagus elephas (Orthoptera: Pamphagidae) has been analysed by gas chromatography and by combined gas chromatograph-mass spectrometry. The following hydrocarbon classes have been identified in insect cuticular hydrocarbons are: n-alkanes and methylalkanes comprising Monomethyl-, dimethyl-and trimethylalkanes. Sexual dimorphism is observed in long chain alkanes (C24-C36) present on male and female. The cuticulars hydrocarbons of P.elephas ranged from 24 to 36 carbons and incluted n-alkanes, Dimethylalkanes and Trimethylalkanes. nalkanes represented by (C24-C36,72,7% on male and 79,2% on female), internally branched Monomethylalkanes identified were (C25, C30-C32,C35-C37;11% on male and 9,4% on female), Dimethylalkanes detected are (C31-C32, C36; 2,2% on male and 2,06% on female) and Trimethylalkanes detected are (C32, C36; 3,1% on male and 4, 97 on female). Larvae male and female (stage 7) showed the same quality of n-alkanes observed in adults. However a difference quantity is noted.

Keywords: Cuticular hydrocarbons, Gas chromatography, Mass spectrometry, Pamphagus elephas, , Sexual dimorphism

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Authors: Y. L. Yung, Kong Mun Lo

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In this study, solid phase micro-extraction (SPME) was optimized to improve the sensitivity and accuracy in formaldehyde determination for plywood panels. Further work has been carried out to compare the newly developed technique with existing method which reacts formaldehyde collected in desiccators with acetyl acetone reagent (DC-AA). In SPME, formaldehyde was first derivatized with O-(2,3,4,5,6 pentafluorobenzyl)-hydroxylamine hydrochloride (PFBHA) and analysis was then performed by gas chromatography in combination with mass spectrometry (GC-MS). SPME data subjected to various wood species gave satisfactory results, with relative standard deviations (RSDs) obtained in the range of 3.1-10.3%. It was also well correlated with DC values, giving a correlation coefficient, RSQ, of 0.959. The quantitative analysis of formaldehyde by SPME was an alternative in wood industry with great potential

Keywords: Formaldehyde, GCMS, Plywood and SPME

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

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Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

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Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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Authors: Dije Dehari, Ahmed Jashari, Shefket Dehari, Agim Shabani

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New complexes of nickel (II) have been synthesized in the reaction mixture of nickel (II) acetate and 4-hydroxy-2-oxo-2H-chromene-3-carboxamide. Bis(4-hydroxy-2-oxo-2H-chromene-3-carboxamidato-O,O)nickel (II) and diaquabis(4-hydroxy-2-oxo-2H-chromene-3-carboxamidato-O,O)nickel (II) were characterized by elemental analysis, IR spectroscopy and ESI mass spectrometry. Elemental analysis and mass spectrometry data of the complexes suggests the stoichiometry of 1:2 (metal-ligand).

Keywords: Nickel complexes, 4-hydroxy-2-oxo-2H-chromene-3-carboxamide, IR spectroscopy, mass spectrometry.

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Authors: Ayat Bani Rashaid, Zain Khasawneh, Mazin Alqhazo, Shreen Nusair, Mohammad El-Khateeb, Mahmoud Bashtawi

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Autism Spectrum disorder (ASD) is a psychiatric disorder with unknown etiology that mainly affects children in the first three years of life. Alterations of amino acid levels are believed to contribute to ASD. The levels of six essential amino acids (methionine, histidine, valine, leucine, threonine, and phenylalanine), five conditional amino acids (proline, tyrosine, glutamine, cysteine, and cystine), and five non-essential amino acids (asparagine, aspartic acid, alanine, serine, and glutamic acid) in hair samples of children with ASD (n = 25) were analyzed and compared to corresponding levels in healthy age-matched controls (n = 25). The results showed that the levels of methionine, alanine, and asparagine were significantly lower in the hair samples of ASD group compared to those of the control group (p ≤ 0.05). However, the levels of glutamic acid were significantly higher in the ASD group than the control group (p ≤ 0.05). The current findings could contribute towards further understanding of ASD etiology and provide specialists with a hair amino acid profile utilized as a biomarker for early diagnosis of ASD. Such biomarkers could participate in future developments of therapies that reduce ASD-related symptoms.

Keywords: Autism spectrum disorder, amino acids, liquid chromatography-tandem mass spectrometry, human hair.

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Authors: Isam A. Mohamed Ahmed, Jiro Arima, Tsuyoshi Ichiyanagi, Emi Sakuno, Nobuhiro Mori

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The aim of this study was to screen for microorganism that able to utilize 3-N-trimethylamino-1-propanol (homocholine) as a sole source of carbon and nitrogen. The aerobic degradation of homocholine has been found by a gram-positive Rhodococcus sp. bacterium isolated from soil. The isolate was identified as Rhodococcus sp. strain A4 based on the phenotypic features, physiologic and biochemical characteristics, and phylogenetic analysis. The cells of the isolated strain grown on both basal-TMAP and nutrient agar medium displayed elementary branching mycelia fragmented into irregular rod and coccoid elements. Comparative 16S rDNA sequencing studies indicated that the strain A4 falls into the Rhodococcus erythropolis subclade and forms a monophyletic group with the type-strains of R. opacus, and R. wratislaviensis. Metabolites analysis by capillary electrophoresis, fast atom bombardment-mass spectrometry, and gas chromatography- mass spectrometry, showed trimethylamine (TMA) as the major metabolite beside β-alanine betaine and trimethylaminopropionaldehyde. Therefore, the possible degradation pathway of trimethylamino propanol in the isolated strain is through consequence oxidation of alcohol group (-OH) to aldehyde (-CHO) and acid (-COOH), and thereafter the cleavage of β-alanine betaine C-N bonds yielded trimethylamine and alkyl chain.

Keywords: Homocholine, 3-N-trimethylamino-1-propanol, Quaternary ammonium compounds, 16S rDNA gene sequence.

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Authors: Santanu Ray, Alexander G. Shard

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The adsorption of bovine serum albumin (BSA), immunoglobulin G (IgG) and fibrinogen (Fgn) on fluorinated selfassembled monolayers have been studied using time of flight secondary ion mass spectrometry (ToF-SIMS) and Spectroscopic Ellipsometry (SE). The objective of the work has to establish the utility of ToF-SIMS for the determination of the amount of protein adsorbed on the surface. Quantification of surface adsorbed proteins was carried out using SE and a good correlation between ToF-SIMS results and SE was achieved. The surface distribution of proteins were also analysed using Atomic Force Microscopy (AFM). We show that the surface distribution of proteins strongly affect the ToFSIMS results.

Keywords: ToF-SIMS, Spectroscopic Ellipsometry, Protein, Atomic Force Microscopy.

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Authors: A. Aljohani, M. Orif

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The concentration of polycyclic aromatic hydrocarbons (PAH) in clams (A. glabrata) was examined in samples collected from Alseef Beach, 30 km south of Jeddah city. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the 14 PAHs. The concentration of total PAHs was found to range from 11.521 to 40.149 ng/gdw with a mean concentration of 21.857 ng/gdw, which is lower compared to similar studies. The lower molecular weight PAHs with three rings comprised 18.14% of the total PAH concentrations in the clams, while the high molecular weight PAHs with four rings, five rings, and six rings account for 81.86%. Diagnostic ratios for PAH source distinction suggested pyrogenic or anthropogenic sources.

Keywords: Bivalves, biomonitoring, hydrocarbons, PAHs.

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Authors: S. Lakestani, B. Karakas, S. Acar Vaizoglu, B. Guciz Dogan, C. Guler, B. Sekerel, A. Taner, G. Gullu

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Abstract–Indoor air (VOCs) samples were collected simultaneously from variety of indoors (e.g. living rooms, baby-s rooms) and outdoor environments which were voluntarily selected from the houses in which pregnant residents live throughout Ankara. This is the first comprehensive study done in Turkey starting from prenatal period and continued till the babies had one year old. VOCs levels were measured over 76 homes. Air samples were collected in Tenax TA sorbent filled tubes with active sampling method and analyzed with Thermal Desorber and Gas Chromatography/Mass spectrometry (TD-GC/MS). At the first sampling period in the baby-s rooms maximum concentration of toluene was measured about 240.77μg.m-3 and in the living rooms maximum concentration of naphthalene was 180.24μg.m-3. At the second sampling period in the baby-s rooms maximum concentration of toluene was measured about 144.97μg.m-3 and in the living rooms maximum concentration of naphthalene was 247.89μg.m-3. Concentration of TVOCs in the first period was generally higher than the second period.

Keywords: Indoor Air, Volatile Organic Compounds (VOCs), Gas Chromatography

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Authors: Carlos Huertas, Reyes Juarez-Ramirez

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Public health is one of the most critical issues today; therefore, there is great interest to improve technologies in the area of diseases detection. With machine learning and feature selection, it has been possible to aid the diagnosis of several diseases such as cancer. In this work, we present an extension to the Heat Map Based Feature Selection algorithm, this modification allows automatic threshold parameter selection that helps to improve the generalization performance of high dimensional data such as mass spectrometry. We have performed a comparison analysis using multiple cancer datasets and compare against the well known Recursive Feature Elimination algorithm and our original proposal, the results show improved classification performance that is very competitive against current techniques.

Keywords: Feature selection, mass spectrometry, biomarker discovery, cancer.

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Authors: K. J. Sannapapamma, H. Malligawad Lokanath, Sakeena Naikwadi

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Eco-friendly textiles are gaining importance among the consumers and textile manufacturers in the healthcare sector due to increased environmental pollution which leads to several health and environmental hazards. Hence, the research was designed to cultivate and develop the organic cotton knit, to prepare and characterize the Vetiver oil microcapsules for textile finishing and to access the wash durability of finished knits. The cotton SAHANA variety grown under organic production systems was processed and spun into 30 single yarn dyed with four natural colorants (Arecanut slurry, Eucalyptus leaves, Pomegranate rind and Indigo) and eco dyed yarn was further used for development of single jersy knitted fabric. Vetiveria zizanioides is an aromatic grass which is being traditionally used in medicine and perfumery. Vetiver essential oil was used for preparation of microcapsules by interfacial polymerization technique subjected to Gas Chromatography Mass Spectrometry (GCMS), Fourier Transform Infrared Spectroscopy (FTIR), Thermo Gravimetric Analyzer (TGA) and Scanning Electron Microscope (SEM) for characterization of microcapsules. The knitted fabric was finished with vetiver oil microcapsules by exhaust and pad dry cure methods. The finished organic knit was assessed for laundering on antimicrobial efficiency and aroma intensity. GCMS spectral analysis showed that, diethyl phthalate (28%) was the major compound found in vetiver oil followed by isoaromadendrene epoxide (7.72%), beta-vetivenene (6.92%), solavetivone (5.58%), aromadenderene, azulene and khusimol. Bioassay explained that, the vetiver oil and diluted vetiver oil possessed greater zone of inhibition against S. aureus and E. coli than the coconut oil. FTRI spectra of vetiver oil and microcapsules possessed similar peaks viz., C-H, C=C & C꞊O stretching and additionally oil microcapsules possessed the peak of 3331.24 cm^-1 at 91.14 transmittance was attributed to N-H stretches. TGA of oil microcapsules revealed that, there was a minimum weight loss (5.835%) recorded at 467.09°C compared to vetiver oil i.e., -3.026% at the temperature of 396.24°C. The shape of the microcapsules was regular and round, some were spherical in shape and few were rounded by small aggregates. Irrespective of methods of application, organic cotton knits finished with microcapsules by pad dry cure method showed maximum zone of inhibition compared to knits finished by exhaust method against S. aureus and E. coli. The antimicrobial activity of the finished samples was subjected to multiple washing which indicated that knits finished with pad dry cure method showed a zone of inhibition even after 20^th wash and better aroma retention compared to knits finished with the exhaust method of application. Further, the group of respondents rated that the 5^th washed samples had the greater aroma intensity in both the methods than the other samples. Thus, the vetiver microencapsulated organic cotton knits are free from hazardous chemicals and have multi-functional properties that can be suitable for medical and healthcare textiles.

Keywords: Exhaust and pad dry cure finishing, interfacial polymerization, organic cotton knits, vetiver oil microcapsules.

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Authors: D. Mohd Nazrul Hisham, J. Mohd Lip, R. Suri, H. Mohamed Shafit, Z.Kharis, K. Shazlin, A. Normah, M.F. Nurul Nabilah

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Presence of phytosterol compound in Durian seed (Durio zibethinus) or known as King of fruits has been discovered from screening work using reagent test. Further analysis work has been carried out using mass spectrometer in order to support the priliminary finding. Isolation and purification of the major phytosterol has been carried out using an open column chromatography. The separation was monitored using thin layer chromatography (TLC). Major isolated compounds and purified phytosterol were identified using mass spectrometer and nuclear magnetic resonance (NMR). This novel finding could promote utilization of durian seeds as a functional ingredient in food products through production of standardized extract based on phytosterol content.

Keywords: Agrowaste, durian, seed, phytosterol

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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: Mohanad El-Harbawi, Nurul Amirah Hanim Bt. Umar, Norizan Ali, Yoshimitsu Uemura

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Study of fire and explosion is very important mainly in oil and gas industries due to several accidents which have been reported in the past and present. In this work, we have investigated the flammability of bio oil vapour mixtures. This mixture may contribute to fire during the storage and transportation process. Bio oil sample derived from Palm Kernell shell was analysed using Gas Chromatography Mass Spectrometry (GC-MS) to examine the composition of the sample. Mole fractions of 12 selected components in the liquid phase were obtained from the GC-FID data and used to calculate mole fractions of components in the gas phase via modified Raoult-s law. Lower Flammability Limits (LFLs) and Upper Flammability Limits (UFLs) for individual components were obtained from published literature. However, stoichiometric concentration method was used to calculate the flammability limits of some components which their flammability limit values are not available in the literature. The LFL and UFL values for the mixture were calculated using the Le Chatelier equation. The LFLmix and UFLmix values were used to construct a flammability diagram and subsequently used to determine the flammability of the mixture. The findings of this study can be used to propose suitable inherently safer method to prevent the flammable mixture from occurring and to minimizing the loss of properties, business, and life due to fire accidents in bio oil productions.

Keywords: Gas chromatography, compositions, lower and upper flammability limits (LFL & UFL), flammability diagram.

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Authors: Gaurav Bhanjana, Ganga Ram Chaudhary, Sandeep Kumar, Neeraj Dilbaghi

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Main sources of endocrine disrupting compounds in the ecosystem are hormones, pesticides, phthalates, flame retardants, dioxins, personal-care products, coplanar polychlorinated biphenyls (PCBs), bisphenol A, and parabens. These endocrine disrupting compounds are responsible for learning disabilities, brain development problems, deformations of the body, cancer, reproductive abnormalities in females and decreased sperm count in human males. Although discharge of these chemical compounds into the environment cannot be stopped, yet their amount can be retarded through proper evaluation and detection techniques. The available techniques for determination of these endocrine disrupting compounds mainly include high performance liquid chromatography (HPLC), mass spectroscopy (MS) and gas chromatography-mass spectrometry (GC–MS). These techniques are accurate and reliable but have certain limitations like need of skilled personnel, time consuming, interference and requirement of pretreatment steps. Moreover, these techniques are laboratory bound and sample is required in large amount for analysis. In view of above facts, new methods for detection of endocrine disrupting compounds should be devised that promise high specificity, ultra sensitivity, cost effective, efficient and easy-to-operate procedure. Nowadays, electrochemical sensors/biosensors modified with nanomaterials are gaining high attention among researchers. Bioelement present in this system makes the developed sensors selective towards analyte of interest. Nanomaterials provide large surface area, high electron communication feature, enhanced catalytic activity and possibilities of chemical modifications. In most of the cases, nanomaterials also serve as an electron mediator or electrocatalyst for some analytes.

Keywords: Sensors, endocrine disruptors, nanoparticles, electrochemical, microscopy.

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Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

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This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, ¹H and ¹³C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]⁺ peaks at m/z 312, which are in agreement to the calculated molecular weight. For ¹H NMR spectra, the presence of OCH₃, C=S-NH and C=O-NH protons were observed within range of δ_H 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. ¹³C NMR spectra in all compounds displayed the presence of OCH₃, C=O-NH, C=O-OH and C=S carbon resonances within range of δ_C 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm^-1, 2976-3302 cm^-1, 1720-1768 cm^-1, 1655-1672 cm^-1, 1519-1525 cm^-1 and 754-763 cm^-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: Methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial.

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Authors: Ji Young Song, Soo Jung Hu, Hyunjin Joo, Joung Boon Hwang, Mi Ok Kim, Shin Jung Kang, Dae Hyun Cho

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Multi-residue analysis method for penicillins was developed and validated in bovine muscle, chicken, milk, and flatfish. Detection was based on liquid chromatography tandem mass spectrometry (LC/MS/MS). The developed method was validated for specificity, precision, recovery, and linearity. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin (59.7%). Relative standard deviations (RSDs) were not more than 10%. LOQs values ranged from 0.1 and to 4.5 ug/kg. The method was applied to 128 real samples. Benzylpenicillin was detected in 15 samples and Cloxacillin was detected in 7 samples. Oxacillin was detected in 2 samples. But the detected levels were under the MRL levels for penicillins in samples.

Keywords: Penicillins, livestock product, Multi-residue analysis, LC/MS/MS

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Authors: M. Hakami, A. Jammaly, I. Attafi, M. Oraiby, M. Jeraiby

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We reviewed an unusual case of a 65-year-old male taking an herbal mixture containing compounds with anticholinesterase activity for a long period of time, presented with acute my myocardial infarction and multiple organ dysfunction syndrome followed by death. Clinically, there are findings correlated with anticholinesterase activity, such as bilateral miosis, diaphoresis, vomiting and fasciculation without a history of any toxic ingestion or exposure. Gas chromatography–mass spectrometry screening studies identified the presence of thymol, anethole in the herbal extract and butylated hydroxytoluene in the blood sample. Hence, with this case report, we intend to highlight the necessity of evaluating the long-term use of the herbal mixture.

Keywords: Cholinesterase inhibitors, thymol, anethole, butylated hydroxytoluene, cardiac toxicity and myocardial infarction.

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Authors: D. S. Fardhyanti, A. Damayanti

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Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kinds 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. 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 are 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: Y. T. Boon, M. N. Naim, R. Zakaria, N. F. Abu Bakar, N. Ahmad, I. W. Lenggoro

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In this study, encapsulation of agarwood oil with non-ionic surfactant, Tween 80 was prepared at critical micelle concentration of 0.0167 % v/v to produce the most stable nano-emulsion in aqueous. The encapsulation has minimized the bioactive compounds degradation in various pH conditions thus prolong their shelf life and maintained its initial oil grade. The oil grading of the prepared samples were conducted using the gel electrophoresis instead of using common analytical industrial grading such as gas chromatography- mass spectrometry (GC- MS). The grading method was chosen due to their unique zeta potential value after the encapsulation process. This paper demonstrates the feasibility of applying the electrophoresis principles to separate the encapsulated agarwood oil or grading of the emulsified agarwood oil. The results indicated that the grading process are potential to be further investigate based on their droplet size and zeta potential value at various pH condition when the droplet were migrate through polyacrylamide gel.

Keywords: Electrophoretic mobility, essential oil, nanoemulsion, polyacrylamide gel electrophoresis, Tween 80, zeta potential.

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Authors: M. O. Ezegbogu, H. B. Osadolor

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Lipsticks constitute a significant source of transfer evidence, and can, therefore, provide corroborative or inclusionary evidence in criminal investigation. This study aimed to determine the uniqueness and persistence of different lipstick smears using Thin Layer Chromatography (TLC), and Gas Chromatography with a Flame Ionisation Detector (GC-FID). In this study, we analysed lipstick smears retrieved from tea cups exposed to the environment for up to four weeks. The n-alkane content of each sample was determined using GC-FID, while TLC was used to determine the number of bands, and retention factor of each band per smear. This study shows that TLC gives more consistent results over a 4-week period than GC-FID. It also proposes a maximum exposure time of two weeks for the analysis of lipsticks left in the open using GC-FID. Finally, we conclude that neither TLC nor GC-FID can distinguish lipstick evidence recovered from hypothetical crime scenes.

Keywords: Forensic science, chromatography, identification, lipstick.

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Authors: N. B. Dhayanithi, T. T. Ajith Kumar, T. Balasubramanian

Abstract:

Present study summarizes the control of Vibrio alginolyticus infection in hatchery reared Clownfish, Amphiprion sebae with the extract of the mangrove plant, Avicennia marina. Fishes with visible symptoms of hemorrhagic spots were chosen and the genomic DNA of the causative bacterium was isolated and sequenced based on 16S rDNA gene. The in vitro assay revealed that a fraction of A. marina leaf extract elucidated with ethyl acetate: methanol (6:4) showed a high activity (28 mm) at 125 μg/ml concentrations. About 4 % of the fraction fed along with live V. alginolyticus was significantly decreased the cumulative mortality (P<0.05) in the experimental groups than the control group. The responsible fraction was investigated by gas chromatography - mass spectroscopy and found the presence of active compounds. This is the first research in India to control vibriosis infection in marine ornamental fish with mangrove leaf extract.

Keywords: Amphiprion seabe, Avicennia marina, Gas Chromatography - Mass Spectroscopy, Vibrio alginolyticus

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Authors: John R. Rose, James P. Cleveland, Alvin Fox

Abstract:

Tandem mass spectrometry (MS/MS) is the engine driving high-throughput protein identification. Protein mixtures possibly representing thousands of proteins from multiple species are treated with proteolytic enzymes, cutting the proteins into smaller peptides that are then analyzed generating MS/MS spectra. The task of determining the identity of the peptide from its spectrum is currently the weak point in the process. Current approaches to de novo sequencing are able to compute candidate peptides efficiently. The problem lies in the limitations of current scoring functions. In this paper we introduce the concept of proteome signature. By examining proteins and compiling proteome signatures (amino acid usage) it is possible to characterize likely combinations of amino acids and better distinguish between candidate peptides. Our results strongly support the hypothesis that a scoring function that considers amino acid usage patterns is better able to distinguish between candidate peptides. This in turn leads to higher accuracy in peptide prediction.

Keywords: Tandem mass spectrometry, proteomics, scoring, peptide, de novo, mutual information

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Authors: So-young Jung, Bu-chuhl Choe, Gi-young Shin, Jung-hun Kim, Young-zoo Chae

Abstract:

A sensitive and specific method for quantitative determination of aflatoxins(B1, B2, G1,G2), deoxynivalenol, fumonisin(B1,B2), ochratoxin A, zearalenone, T-2 and HT-2 in roasted and ground grains using liquid chromatography combined with tandem mass spectrometry. A double extraction using a phosphate buffer solution followed by methanol was applied to achieve effective co extraction of 11 mycotoxins. A multitoxin immunoaffinity column for all these mycotoxins was used to clean up the extract. The LODs of mycotoxins were 0.1~6.1 μg/kg, LOQs were 0.3~18.4 μg/kg. Forty seven samples collected from Seoul (Korea) for mycotoxin contamination monitoring. The results showed that the occurrence of zearalenone and deoxynivalenol were frequent. Zearalenone was detected in all samples and deoxynivalenol was detected in 80.9 % samples in the range 0.626 ~ 29.264 μg/kg and N.D ~ 48.332 μg/kg respectively. Fumonisins and ochratoxin A were detected in 46.8% samples and 17 % samples respectively, aflatoxins and T-2/HT-2 toxins were not detected all samples.

Keywords: LC-MS/MS, mycotoxins, roasted and ground grains.

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Authors: F. Benkaci-Ali, R. Mekaoui, G. Eppe, E. De Pau, J. F. Faucont

Abstract:

Team distillation assisted by microwave extraction (SDAM) considered as accelerated technique extraction is a combination of microwave heating and steam distillation, performed at atmospheric pressure. SDAM has been compared with the same technique coupled with the cryogrinding of seeds (SDAM -CG). Isolation and concentration of volatile compounds are performed by a single stage for the extraction of essential oil from Cuminum cyminum seeds. The essential oils extracted by these two methods for 5 min were quantitatively (yield) and qualitatively (aromatic profile) no similar. These methods yield an essential oil with higher amounts of more valuable oxygenated compounds, and allow substantial savings of costs, in terms of time, energy and plant material. SDAM and SDAM-CG is a green technology and appears as a good alternative for the extraction of essential oils from aromatic plants.

Keywords: Steam distillation, microwave extraction, Cuminum cyminum, chromatography, mass spectrometry

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Authors: A. Belhaj Mohamed, M. Saidi, N. Boucherb, N. Ourtani, A. Soltani, I. Bouazizi, M. Ben Jrad

Abstract:

Natural hydrocarbon seepage has helped petroleum exploration as a direct indicator of gas and/or oil subsurface accumulations. Surface macro-seeps are generally an indication of a fault in an active Petroleum Seepage System belonging to a Total Petroleum System. This paper describes a case study in which multiple analytical techniques were used to identify and characterize trace petroleum-related hydrocarbons and other volatile organic compounds in groundwater samples collected from Sousse aquifer (Central Tunisia). The analytical techniques used for analyses of water samples included gas chromatography-mass spectrometry (GCMS), capillary GC with flame-ionization detection, Compound Specific Isotope Analysis, Rock Eval Pyrolysis. The objective of the study was to confirm the presence of gasoline and other petroleum products or other volatile organic pollutants in those samples in order to assess the respective implication of each of the potentially responsible parties to the contamination of the aquifer. In addition, the degree of contamination at different depths in the aquifer was also of interest. The oil and gas seeps have been investigated using biomarker and stable carbon isotope analyses to perform oil-oil and oil-source rock correlations. The seepage gases are characterized by high CH4 content, very low δ13CCH4 values (-71,9 ‰) and high C1/C1–5 ratios (0.95–1.0), light deuterium–hydrogen isotope ratios (- 198 ‰) and light δ13CC2 and δ13CCO2 values (-23,8‰ and-23,8‰ respectively) indicating a thermogenic origin with the contribution of the biogenic gas. An organic geochemistry study was carried out on the more ten oil seep samples. This study includes light hydrocarbon and biomarkers analyses (hopanes, steranes, n-alkanes, acyclic isoprenoids, and aromatic steroids) using GC and GC-MS. The studied samples show at least two distinct families, suggesting two different types of crude oil origins: the first oil seeps appears to be highly mature, showing evidence of chemical and/or biological degradation and was derived from a clay-rich source rock deposited in suboxic conditions. It has been sourced mainly by the lower Fahdene (Albian) source rocks. The second oil seeps was derived from a carbonate-rich source rock deposited in anoxic conditions, well correlated with the Bahloul (Cenomanian-Turonian) source rock.

Keywords: Biomarkers, oil and gas seeps, organic geochemistry, source rock.

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