Paraquat poisoning is commonly associated with suicide or homicide in Malaysia. In a case involving advanced body decomposition, pathological analysis regarding the cause of death may become difficult or almost impossible. Insects serve as common alternative matrix for poison detection in forensic analysis. Paraquat detection via secondary bioaccumulation in fly larvae tissue has never been reported. In this study, tissues from blowfly larvae collected from a rabbit carcass with paraquat poisoning were analyzed for secondary bioaccumulation. Larvae samples were collected and analyzed using liquid-liquid extraction. The detection was performed via reduction of quaternary ammonium presence in paraquat and analyzed using gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring mode (SIM mode). GC-MS showed the elution of reduced paraquat was at retention time 12.8 min. Blowfly larvae tissue has proven useful as a secondary detector in paraquat-related deaths.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
A sensitive and selective gas chromatography with mass spectrometry method was developed for the simultaneous determination of three organophosphorus pesticides, namely, chlorpyrifos, malathion, and diazinon in three different food commodities (milk, apples, and drinking water) employing solid-phase extraction for sample pretreatment. Pesticide extraction from different sample matrices was carried out on Chromabond C18 cartridges using 3.0 mL of methanol and 3.0 mL of a mixture of dichloromethane/acetonitrile (1:1 v/v) as the eluting solvent. Analysis was carried out by gas chromatography coupled with mass spectrometry using selected-ion monitoring mode. Good linear relationships were obtained in the range of 0.1-50 μg/L for chlorpyrifos, and 0.05-50 μg/L for both malathion and diazinon pesticides. Good repeatability and recoveries were obtained in the range of 78.54-86.73% for three pesticides under the optimized experimental conditions. The limit of detection ranged from 0.02 to 0.03 μg/L, and the limit of quantification ranged from 0.05 to 0.1 μg/L for all three pesticides. Finally, the developed method was successfully applied for the determination of three targeted pesticides in milk, apples, and drinking water samples each in triplicate. No pesticide was found in apple and milk samples, but chlorpyrifos was found in one drinking water sample below the quantification level.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Cryptococcus neoformans is an encapsulated basidiomycetous yeast commonly associated with pigeon droppings and soil. The opportunistic pathogen infects humans through the respiratory system and the metabolic implications of C. neoformans infection have yet to be explored. Studying the metabolic profile associated with the infection could lead to the identification of important metabolites associated with pulmonary infection. Therefore, the aim of the study was to simulate cryptococcal infection at the primary site of infection, the lungs, and to identify the metabolic profile and important metabolites associated with the infection at low and high multiplicity of infections (MOI). The culture supernatant of lung epithelial cells infected with C. neoformans at MOI of 10 and 100 over a period of 18 hours were analysed using gas chromatography mass spectrometry. The metabolic profiles obtained were further analysed using multivariate analysis and the pathway analysis tool, MetaboAnalyst 2.0. Based on the results from the multivariate analyses, ten metabolites were selected as the discriminatory metabolites that were important in both the infection conditions. The pathways affected during early C. neoformans infection of lung epithelial cells were mainly the central carbon metabolism and biosynthesis of amino acids. Infection at a higher MOI led to a perturbance in the β-alanine metabolism and an increase in the secretion of pantothenic acid into the growth media. Pantothenic acid production during yeast infection has not been documented and the β-alanine metabolism as well as the pantothenate and CoA biosynthesis pathways may represent underlying metabolic pathways associated with disease progression. Our study suggested that β-alanine metabolism and the pantothenate and CoA biosynthesis pathways might be the important pathways associated with cryptococcal infection.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Methyl esters from vegetable oils have attracted a great deal of interest as substitute for petrodiesel to reduce dependence on imported petroleum and provide an alternate and sustainable source for fuel with more benign environmental properties. In the present study biodiesel was prepared from sunflower seed oil by transesterification by alkali-catalyzed methanolysis. The fuel properties of sunflower oil biodiesel were determined and discussed in the light of ASTM D6751 standards for biodiesel. The sunflower oil biodiesel was chemically characterized with analytical techniques like FT-IR, and NMR ((1)H and (13)C). The chemical composition of sunflower oil biodiesel was determined by GC-MS. Various fatty acid methyl esters (FAMEs) were identified by retention time data and verified by mass fragmentation patterns. The percentage conversion of triglycerides to the corresponding methyl esters determined by (1)H NMR was 87.33% which was quite in good agreement with the practically observed yield of 85.1%.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
This paper examines the processing steps of extracting palm oil from fresh fruit bunches in a way that may impact on the formation of chloropropandiol fatty esters (3-MCPD esters), particularly during refining. Diacylglycerols (DAGs) do not appear to be a critical factor when crude palm oils are extracted from various qualities of fruit bunches. Highly hydrolysed oils, in spite of the high free fatty acid (FFA) contents, did not show exceptionally high DAGs, and the oils did not display a higher formation of 3-MCPD esters upon heat treatment. However, acidity measured in terms of pH appears to have a strong impact on 3-MCPD ester formation in the crude oil when heated at high temperatures. The differences in the extraction process of crude palm oil from current commercial processes and that from a modified experimental process showed clearly the effect of acidity of the oil on the formation of 3-MCPD esters. This paper concludes that the washing or dilution step in palm oil mills removes the acidity of the vegetative materials and that a well-optimised dilution/washing step in the extraction process will play an important role in reducing formation of 3-MCPD esters in crude palm oil upon further heat processing.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Salbutamol ¿2-(tert-butylamino)-1-[4-hydroxy-3- (hydroxymethyl)phenyl]ethanol¿, also known as albuterol, is clinically the most widely used beta 2-adrenoceptor agonist in the treatment of bronchial asthma. During this study, we evaluated liquid-liquid extraction (LLE) and solid-phase extraction (SPE) in order to develop a reliable extraction method followed by analysis using liquid chromatography and gas chromatography. An assay is described which involves SPE as the clean-up method followed by gas chromatography-mass spectrometry to determine salbutamol levels in human serum after oral administration. The SPE method requires the use of a hyper-cross-linked styrene-divinylbenzene bonded phase (ENV+) without involving any sample pre-treatment to obtain 60-65% recoveries for salbutamol and terbutaline as the internal standard. Distilled water and 1% trifluoroacetic acid in methanol were found to be the most suitable washing solvent and eluting solvent, respectively. A detection limit of 2 ng mL-1 was achieved by derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide to form trimethylsilyl (TMS)-salbutamol (m/z 369) and TMS-terbutaline (m/z 356). The relationship between the ratio of the peak area of salbutamol to that of the internal standard and concentration was linear for the range tested (2-200 ng mL-1) and the correlation of coefficient was 0.9999 with a y-intercept not significantly different from zero. The inter-day relative standard deviation (RSD) was < 10% for all three concentrations. The intra-day RSD was 14% for 2 ng mL-1. This assay was then successfully applied to human serum samples obtained from clinical trials after oral administration of salbutamol.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Leaf extracts of Callicarpa pentandra provided four new clerodane-type diterpenoids (1-4), of which 1, 2, and 4 have ring-A-contracted structures. Their structures and stereochemistry were established by spectral data interpretation, and for 3 also by single-crystal X-ray diffraction.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Spectroscopic examinations of purified extracts of the rumen content of sheep intoxicated by Brachiaria decumbens revealed the presence of a mixture of sapogenins, identified as 3-spirostanols. These isomeric steroid sapogenins (C27H44O3) are believed the toxic principles in causing toxicity in sheep after feeding on B. decumbens.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
The haze episodes that occurred in Malaysia in September-October 1991, August-October 1994 and September-October 1997 have been attributed to suspended smoke particulate matter from biomass burning in southern Sumatra and Kalimantan, Indonesia. In the present study, polar organic compounds in aerosol particulate matter from Malaysia are converted to their trimethylsilyl derivatives and analyzed by gas chromatography-mass spectrometry in order to better assess the contribution of the biomass burning component during the haze episodes. On the basis of this analysis, levoglucosan was found to be the most abundant organic compound detected in almost all samples. The monosaccharides, alpha- and beta-mannose, the lignin breakdown products, vanillic and syringic acids and the minor steroids, cholesterol and beta-sitosterol were also present in some samples. The presence of the tracers from smoke overwhelmed the typical signatures of emissions from traffic and other anthropogenic activities in the urban areas.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Natural products have demonstrated various activities beneficial to general health. Flaxseed (Linum usitatissimum) has been reported in many studies for its antimicrobial, antioxidant, and anti-inflammatory effects. Additionally, flaxseed extracts have skin wound healing activity and potential for treating oral ulcers.L. usitatissimum was extracted using 70% ethanol via soxhlet method and gas chromatography mass spectrum (GC-MS) was used to analyze the components of L. usitatissimum extract. The crude flaxseed oil were applied to human oral fibroblasts (HOrF), and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) assay was used to assess the cell viability after 24, 48 and 72 hours. Scratched HOrF cells were treated with crude flaxseed oil and healing was monitored per wound healing assay. GC-MS indicate that the major components present in L. usitatissimum oil extract are linolic, palmitic and oleic acid. L. usitatissimum crude oil extract showed high proliferation effect on HOrF cells at 24 and 48 hours, while the highest proliferation effect was recorded at 72 hours post-treatment. The wound healing assay results showed that healing activity of HOrF cells occurred as soon as 18 hours post-treatment when treated with L. usitatissimum crude oil extract. L. usitatissimum crude oil extract has proliferating and healing effects on HOrF cell line. Therefore, it can be considered as a potential promising oral wound healing agent.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
This study aimed to determine the distribution and potential health risks of polycyclic aromatic hydrocarbons (PAHs) in PM2.5 collected in Kuala Lumpur during different monsoon seasons. The potential sources of PM2.5 were investigated using 16 priority PAHs with additional of biomass tracers namely levoglucosan (LV), mannosan (MN) and galactosan (GL). This study also investigated the cytotoxic potential of the extracted PAHs towards V79-4 cells. A high-volume air sampler (HVS) was used to collect PM2.5 samples for 24 h. PAHs were extracted using dichloromethane (DCM) while biomass tracers were extracted by a mixture of DCM/methanol (3:1) before analysis with gas chromatography-mass spectrometry (GC-MS). The cytotoxicity of the PAHs extract was determined by assessing the cell viability through the reduction of tetrazolium salts (MTT). The results showed that the total mean ± SD concentrations of PAHs during the southwest (SW) and northeast (NE) monsoons were 2.51 ± 0.93 ng m-3 and 1.37 ± 0.09 ng m-3, respectively. Positive matrix factorization (PMF) using PAH and biomass tracer concentrations suggested four potential sources of PM2.5; gasoline emissions (29.1%), natural gas and coal burning (28.3%), biomass burning (22.3%), and diesel and heavy oil combustion (20.3%). Health risk assessment showed insignificant incremental lifetime cancer risk (ILCR) of 2.40E-07 for 70 years of exposure. MTT assay suggested that PAHs extracts collected during SW monsoon have cytotoxic effect towards V79-4 cell at the concentrations of 25 μg mL-1, 50 μg mL-1, 100 μg mL-1 whereas non-cytotoxic effect was observed on the PAHs sample collected during NE monsoon.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
There are no methods sensitive enough to detect enzymes within cells, without the use of analyte labeling. Here we show that it is possible to detect protein ion signals of three different H2S-synthesizing enzymes inside microglia after pretreatment with silver nanowires (AgNW) using time-of-flight secondary ion mass spectrometry (TOF-SIMS). Protein fragment ions, including the fragment of amino acid (C4H8N+ = 70 amu), fragments of the sulfur-producing cystathionine-containing enzymes, and the Ag+ ion signal could be detected without the use of any labels; the cells were mapped using the C4H8N+ amino acid fragment. Scanning electron microscopy imaging and energy-dispersive X-ray chemical analysis showed that the AgNWs were inside the same cells imaged by TOF-SIMS and transformed chemically into crystalline Ag2S within cells in which the sulfur-producing proteins were detected. The presence of these sulfur-producing cystathionine-containing enzymes within the cells was confirmed by Western blots and confocal microscopy images of fluorescently labeled antibodies against the sulfur-producing enzymes. Label-free TOF-SIMS is very promising for the label-free identification of H2S-contributing enzymes and their cellular localization in biological systems. The technique could in the future be used to identify which of these enzymes are most contributory.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
This study aims to determine the composition of BTEX (benzene, toluene, ethylbenzene and xylene) and assess the risk to health at different sites in Malaysia. Continuous monitoring of BTEX in Kuala Lumpur City Centre, Kuala Terengganu, Kota Kinabalu and Fraser Hill were conducted using Online Gas Chromatograph. For comparison, BTEX at selected hotspot locations were determined by active sampling method using sorbent tubes and Thermal Desorption Gas Chromatography Mass Spectrometry. The hazard quotient (HQ) for non-carcinogenic and the life-time cancer risk (LTCR) of BTEX were calculated using the United States Environmental Protection Agency (USEPA) health risk assessment (HRA) methods. The results showed that the highest total BTEX concentrations using continuous monitoring were recorded in the Kuala Lumpur City Centre (49.56 ± 23.71 μg/m3). Toluene was the most dominant among the BTEX compounds. The average concentrations of benzene ranged from 0.69 ± 0.45 μg/m3 to 6.20 ± 3.51 μg/m3. Measurements using active sampling showed that BTEX concentrations dominated at the roadside (193.11 ± 114.57 μg/m3) in comparison to petrol station (73.08 ± 30.41 μg/m3), petrochemical industry (32.10 ± 13.13 μg/m3) and airport (25.30 ± 6.17 μg/m3). Strong correlations among BTEX compounds (p<0.01, r>0.7) at Kuala Lumpur City Centre showed that BTEX compounds originated from similar sources. The values of HQ at all stations were <1 indicating the non-carcinogenic risk are negligible and do not pose threats to human health. The LTCR value based on benzene inhalation (1.59 × 10-5) at Kuala Lumpur City Centre were between 1 × 10-4 and 1 × 10-5, representing a probable carcinogenic risk.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Different extraction processes were employed to extract bioactive metabolites from Salacca zalacca flesh by a range of aqueous and organic solvents. The highest extraction yield was obtained by 50% ethanol extract of SE (73.18 ± 4.35%), whereas SFE_1 showed the lowest yield (0.42 ± 0.08%). All extracts were evaluated for in vitro α-glucosidase inhibitory activity, measured by their IC50 values in comparison to that of quercetin, the positive control (IC50 = 2.7 ± 0.7 μg/mL). The lowest α-glucosidase inhibitory activity was indicated by water extract of SE (IC50 = 724.3 ± 42.9 μg/mL) and the highest activity was demonstrated by 60% ethanol extract by UAE (IC50 = 16.2 ± 2.4 μg/mL). All extracts were analysed by GC-MS and identified metabolites like carbohydrates, fatty acids, organic acids, phenolic acids, sterols and alkane-based compounds etcetera that may possess the potential as α-glucosidase inhibitor and may attribute to the α-glucosidase inhibitory activity.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Lignin depolymerization for the purpose of synthesizing aromatic molecules is a growing focus of research to find alternative energy sources. In current studies, the photocatalytic depolymerization of lignin has been investigated by two new iso-propylamine-based lead chloride perovskite nanomaterials (SK9 and SK10), synthesized by the facile hydrothermal method. Characterization was done by Powder X-Ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), UV-Visible (UV-Vis), Photoluminescence (PL), and Fourier-Transform Infrared (FTIR) Spectroscopy and was used for the photocatalytic depolymerization of lignin under UV light. Lignin depolymerization was monitored by taking absorption spectra and catalytic paths studied by applying kinetic models. The %depolymerization was calculated for factors such as catalyst dose variation, initial concentration of lignin, and varying temperatures. Pseudo-second order was the best suited kinetic model, exhibiting a mechanism for lignin depolymerization that was chemically rate controlled. The activation energy (Ea) for the depolymerization reaction was found to be 15 kJ/mol, which is remarkably less than conventional depolymerization of the lignin, i.e., 59.75 kJ/mol, exhibiting significant catalytic efficiencies of synthesized perovskites. Products of lignin depolymerization obtained after photocatalytic activity at room temperature (20 °C) and at 90 °C were characterized by GC-MS analysis, indicating an increase in catalytic lignin depolymerization structural subunits into small monomeric functionalities at higher temperatures. Specifically, 2-methoxy-4-methylphenol (39%), benzene (17%), phenol (10%) and catechol (7%) were detected by GC-MS analysis of lignin depolymerization products.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
A biosurfactant-producing and hydrocarbon-utilizing bacterium, Pseudomonas aeruginosa USM-AR2, was used to assist conventional distillation. Batch cultivation in a bioreactor gave a biomass of 9.4 g L(-1) and rhamnolipid concentration of 2.4 g L(-1) achieved after 72 h. Biosurfactant activity (rhamnolipid) was detected by the orcinol assay, emulsification index and drop collapse test. Pretreatment of crude oil TK-1 and AG-2 with a culture of P. aeruginosa USM-AR2 that contains rhamnolipid was proven to facilitate the distillation process by reducing the duration without reducing the quality of petroleum distillate. It showed a potential in reducing the duration of the distillation process, with at least 2- to 3-fold decreases in distillation time. This is supported by GC-MS analysis of the distillate where there was no difference between compounds detected in distillate obtained from treated or untreated crude oil. Calorimetric tests showed the calorie value of the distillate remained the same with or without treatment. These two factors confirmed that the quality of the distillate was not compromised and the incubation process by the microbial culture did not over-degrade the oil. The rhamnolipid produced by this culture was the main factor that enhanced the distillation performance, which is related to the emulsification of hydrocarbon chains in the crude oil. This biotreatment may play an important role to improve the existing conventional refinery and distillation process. Reducing the distillation times by pretreating the crude oil with a natural biosynthetic product translates to energy and cost savings in producing petroleum products.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Considering the importance of tropical almond nuts as a snack item, a study was conducted to identify the flavour volatiles and acrylamide generated during the roasting of the nuts. The supercritical fluid extracted flavour components revealed 74 aroma active compounds made up of 27 hydrocarbons, 12 aldehydes, 11 ketones, 7 acids, 4 esters, 3 alcohols, 5 furan derivatives a pyrazine, and 2 unknown compounds. While low levels of acrylamide (8-86 microg/kg) were obtained in the roasted nuts, significant (P<0.05) increases occurred in concentration with increased roasting temperature and time. Carboxylic acids were the most abundant volatiles in the roasted almond nuts and less significant (P>0.05) concentration of acrylamide was generated with mild roasting and shorter roasting period.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Gracilaria species are red marine macroalgae that are found abundantly in Malaysia. Gracilaria changii from Morib, Selangor, G. nanilaensis and Gracilaria sp. from Gelang Patah, Johor were used in this study. Five compounds were successfully isolated and identified as hexadecanoic acid (1), cholest-5-en-3-ol (2), 2-hydroxymyristic acid (3), cholesteryl myristate (4) and 1-(4'-methoxyphenyl)-3-(2",4",6"-trihydroxyphenyl)-3-hydroxypropanone (5) based on spectral data analysis (IR, UV, GC-MS, 'H NMR, "C NMR, HMQC and HMBC). All compounds isolated were tested for cytotoxicity (MTT assay for HL-60 and MCF-7 cell lines), and antibacterial (disc diffusion method), antioxidant (DPPH free radical scavenging assay and xanthine oxidase inhibitory assay) and acetylcholinesterase inhibitory (AChE) activity (TLC bioautographic method). Compounds I and 3 exhibited strong cytotoxic activity against HL-60 and MCF-7 cell lines. Compound 5 showed high antioxidant activity in both the DPPH free radical scavenging and xanthine oxidase inhibition assays. Compound I showed positive activity for AChE inhibitory with a minimum inhibition dose of 0.625 tg sample. All compounds demonstrated antibacterial activity producing 8 to 14 mm inhibition zones. A positive control was applied to all bioassays and experiments were performed with three replicates. Results demonstrated that three edible red seaweeds are rich sources of bioactive compounds with potential application for pharmaceutical purposes.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fatty acid desaturase catalyzes the desaturation reactions by insertion of double bonds into the fatty acyl chain, producing unsaturated fatty acids. Though soluble fatty acid desaturases have been studied widely in advanced organisms, there are very limited studies of membrane fatty acid desaturases due to the difficulty of generating recombinant desaturase. Brassica napus is a rapeseed, which possesses a range of different membrane-bound desaturases capable of producing fatty acids including Δ3, Δ4, Δ8, Δ9, Δ12, and Δ15 fatty acids. The 1155 bp open reading frame of Δ12 fatty acid desaturase (FAD12) from Brassica napus codes for 383 amino acid residues with a molecular weight of 44 kDa. It was expressed in Escherichia coli at 37 °C in soluble and insoluble forms when induced with 0.5 mM IPTG. Soluble FAD12 has been purified using Ni2+-Sepharose affinity chromatography with a total protein yield of 0.728 mg/mL. Gas chromatography-mass spectrometry (GC-MS) analysis revealed that desaturase activity of FAD12 could produce linoleic acid from oleic acid at a retention time of 17.6 with a conversion rate of 47%. Characterization of purified FAD12 revealed the optimal temperature of FAD12 was 50 °C with 2 mM preferred substrate concentration of oleic acid. Analysis of circular dichroism (CD) showed FAD12 was made up of 47.3% and 0.9% of alpha-helix and β-sheet secondary structures. The predicted Tm value was 50.2 °C.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Averrhoa carambola L. is a tropical tree with edible fruit that grows at different climatic conditions. Despite its nutritive value and reported health benefits, it is a controversial fruit owing to its rich oxalate content. The present study aimed at investigating aroma and nutrient primary metabolites distribution in A. carambola fruits grown in Indonesia, Malaysia (its endemic origin) versus Egypt, and at different ripening stages. Two techniques were employed to assess volatile and non-volatile metabolites including headspace solid-phase micro-extraction (HS-SPME) joined with gas chromatography coupled with mass-spectrometry (GC-MS) and GC-MS post silylation, respectively. Twenty-four volatiles were detected, with esters amounting for the major class of volatiles in Egyptian fruit at ca. 66%, with methyl caproate as the major component, distinguishing it from other origins. In contrast, aldehydes predominated tropically grown fruits with the ether myristicin found exclusively in these. Primary metabolites profiling led to the identification of 117 metabolites viz. sugars, polyols and organic acids. Fructose (38-48%) and glucose (21-25%) predominated sugar compositions in ripe fruits, whereas sorbitol was the major sugar alcohol (2.4-10.5%) in ripe fruits as well. Oxalic acid, an anti-nutrient with potential health risks, was the major organic acid detected in all the studied fruits (1.7-2.7%), except the Malaysian one (0.07%). It increases upon fruit ripening, including considerable amounts of volatile oxalate esters detected via SPME, and which must not be omitted in total oxalate determinations for safety assessments.
Matched MeSH terms: Gas Chromatography-Mass Spectrometry