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Agarose film liquid phase microextraction combined with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in water

Sanagi MM, Loh SH, Wan Ibrahim WA, Hasan MN

J Chromatogr A, 2012 Nov 2;1262:43-8.
PMID: 23021646 DOI: 10.1016/j.chroma.2012.09.007

Agarose film liquid phase microextraction (AF-LPME) procedure for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAHs) in water has been investigated. Agarose film was used for the first time as an interface between donor and acceptor phases in liquid phase microextraction which allowed for selective extraction of the analytes prior to gas chromatography-mass spectrometry. Using 1-octanol as acceptor phase, high enrichment factors in the range of 57-106 for the targeted analytes (fluorene, phenanthrene, fluoranthene and pyrene) were achieved. Under the optimum extraction conditions, the method showed good linearity in the range of 0.1-200 μgL(-1), good correlation coefficients in the range of 0.9963-0.9999, acceptable reproducibility (RSD 6.1-9.2%, n=3), low limits of detection (0.01-0.04 μgL(-1)) and satisfactory relative recoveries (92.9-104.7%). As the AF-LPME device was non-expensive, reuse or recycle of the film was not required, thus eliminating the possibility of analytes carry-over between runs. The AF-LPME technique is environment-friendly and compatible with the green chemistry concept as agarose is biodegradable polysaccharide extracted from seaweed and the procedure requires small volume of organic solvent and generates little waste. The validated method was successfully applied to the analysis of the four analytes in river water samples.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides

Wan Ibrahim WA, Veloo KV, Sanagi MM

J Chromatogr A, 2012 Mar 16;1229:55-62.
PMID: 22326188 DOI: 10.1016/j.chroma.2012.01.022

A novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was produced and applied as sorbent for solid phase extraction (SPE). Five selected organophosphorus pesticides (OPPs) were employed as model compounds to evaluate the extraction performance of the synthesized sol-gel organic-inorganic hybrid MTMOS-TEOS. Analysis was performed using gas chromatography-mass spectrometry. Several important SPE parameters were optimized. Under the optimum extraction conditions, the method using the sol-gel organic-inorganic hybrid MTMOS-TEOS as SPE sorbent showed good linearity in the range of 0.001-1 μg L(-1), good repeatability (RSD 2.1-3.1%, n=5), low limits of detection at S/N=3 (0.5-0.9 pg mL(-1)) and limit of quantification (1-3 pg mL(-1), S/N=10). The performance of the MTMOS-TEOS SPE was compared to commercial C18 Supelclean SPE since C18 SPE is widely used for OPPs. The MTMOS-TEOS SPE method LOD was 500-600 × lower than the LOD of commercial C18 SPE. The LOD achieved with the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent allowed the detection of these OPPs in drinking water well below the level set by European Union (EU) at 0.1 μg L(-1) of each pesticides. The developed MTMOS-TEOS SPE method was successfully applied to real sample analysis of the selected OPPs from several water samples and its application extended to the analysis of several fruits samples. Excellent recoveries and RSDs of the OPPs were obtained from the various water samples (recoveries: 97-111%, RSDs 0.4-2.8%, n=3) and fruit samples (recoveries: 96-111%), RSDs 1-4%, n=5) using the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent. Recoveries and RSDs of OPPs from river water samples and fruit samples using C18 Supelclean SPE sorbent were 91-97%, RSD 0.9-2.6, n=3 and 86-96%, RSD 3-8%, n=5, respectively). The novel sol-gel hybrid MTMOS-TEOS SPE sorbent demonstrate the potential as an alternative inexpensive extraction sorbent for OPPs with higher sensitivity for the OPPs.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Fulltext Gas chromatography-mass spectrometry analysis of various organic extracts of Merremia borneensis from Sabah

Hossain MA, Shah MD, Sakari M

Asian Pac J Trop Med, 2011 Aug;4(8):637-41.
PMID: 21914542 DOI: 10.1016/S1995-7645(11)60162-4

OBJECTIVE: To analyse the chemical composition of different extracts of Merremia borneensis (M. borneensis) by gas chromatography-mass spectrometry (GC-MS).
METHODS: The dried leaves powder was extracted with methanol at room temperature by using Soxhlet extractor. Methanol crude extracts of M. borneensis were extrastel with hexane, chloroform, ethyl acetate and butanol.
RESULTS: Qualitative analyses of various organic crude extracts showed that majority of these are flavonoids, terpeniods, alkaloids and glycosides. Most of the identified compounds by GC-MS are biologically important. Further the M. borneensis leaf possesses certain characteristics that can be ascribed to cultivation on a domestic plantation.
CONCLUSIONS: The suitable extracts for respective compounds can be chosen on the basis of above GC-MS analysis. All the major compounds from different extracts are biologically active molecules. Thus the identification of a good number of compounds from various extracts M. borneensis might have some ecological significance.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Fulltext A biomimetic sensor for the classification of honeys of different floral origin and the detection of adulteration

Zakaria A, Shakaff AY, Masnan MJ, Ahmad MN, Adom AH, Jaafar MN, et al.

Sensors (Basel), 2011;11(8):7799-822.
PMID: 22164046 DOI: 10.3390/s110807799

The major compounds in honey are carbohydrates such as monosaccharides and disaccharides. The same compounds are found in cane-sugar concentrates. Unfortunately when sugar concentrate is added to honey, laboratory assessments are found to be ineffective in detecting this adulteration. Unlike tracing heavy metals in honey, sugar adulterated honey is much trickier and harder to detect, and traditionally it has been very challenging to come up with a suitable method to prove the presence of adulterants in honey products. This paper proposes a combination of array sensing and multi-modality sensor fusion that can effectively discriminate the samples not only based on the compounds present in the sample but also mimic the way humans perceive flavours and aromas. Conversely, analytical instruments are based on chemical separations which may alter the properties of the volatiles or flavours of a particular honey. The present work is focused on classifying 18 samples of different honeys, sugar syrups and adulterated samples using data fusion of electronic nose (e-nose) and electronic tongue (e-tongue) measurements. Each group of samples was evaluated separately by the e-nose and e-tongue. Principal Component Analysis (PCA) and Linear Discriminant Analysis (LDA) were able to separately discriminate monofloral honey from sugar syrup, and polyfloral honey from sugar and adulterated samples using the e-nose and e-tongue. The e-nose was observed to give better separation compared to e-tongue assessment, particularly when LDA was applied. However, when all samples were combined in one classification analysis, neither PCA nor LDA were able to discriminate between honeys of different floral origins, sugar syrup and adulterated samples. By applying a sensor fusion technique, the classification for the 18 different samples was improved. Significant improvement was observed using PCA, while LDA not only improved the discrimination but also gave better classification. An improvement in performance was also observed using a Probabilistic Neural Network classifier when the e-nose and e-tongue data were fused.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods
Identification of thioketone analogues of sildenfil using gas chromatography-mass spectrometry

Man CN, Noor NM, Lajis R

J Chromatogr A, 2011 Sep 28;1218(39):7055-60.
PMID: 21872876 DOI: 10.1016/j.chroma.2011.08.037

Sildenafil analogues have been found adulterated in herbal preparations and food products that claim to have natural aphrodisiacs. In this study, a gas chromatography-mass spectrometry (GC-MS) assay was developed for the screening and identification of thioketone analogues of sildenafil. Thiopyrazolopyrimidine, a precursor or a cleavage product of thioketone analogue, exhibited characteristic fragment ions of m/z 328 and m/z 299 was found to be the best marker to screen the presence of general thioketone analogues. Identification by GC-MS assay was rapid and specific as all the studied thioketones showed characteristic mass fragmentations including their intact molecular ions. The developed GC-MS assay had successfully identified thiosildenafil, thiohomosildenafil and thiodimethylsildenafil in herbal preparation and food products.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Identification of sildenafil, tadalafil and vardenafil by gas chromatography-mass spectrometry on short capillary column

Man CN, Nor NM, Lajis R, Harn GL

J Chromatogr A, 2009 Nov 20;1216(47):8426-30.
PMID: 19853256 DOI: 10.1016/j.chroma.2009.10.016

Sildenafil and its analogues (tadalafil and vardenafil) are phosphodiesterase type 5 inhibitors used in the treatment of male erectile dysfunction. Some dietary supplements, herbal preparations and food products which claim to enhance male sexual function have been found to be adulterated with these drugs. In this study, a gas chromatograph-mass spectrometer (GC-MS) assay was developed for identification of the drugs. In addition to good and short chromatographic separation that can be achieved within 6 min by using a short 10 m capillary column, no prior sample clean-up before GC-MS analysis was required, thus making this assay a cost saving and rapid method. Furthermore, the assay is specific as the identification of sildenafil, tadalafil and vardenafil were done by detection of molecular ions; m/z 474, 389 and 488, [corrected] respectively, and several other characteristic ions resulted from the mass fragmentation of individual molecules. Using our currently developed assay, sildenafil and its analogues were successfully identified in food and herbal matrices.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Anti-Proliferative Effects of Methanol and Water Extracts of Pyrrosia piloselloides on the Hela Human Cervical Carcinoma Cell Line

Sul ‘ain MD, Zakaria F, Johan MF

Asian Pac J Cancer Prev, 2019 Jan 25;20(1):185-192.
PMID: 30678430

Background: Cervical cancer is one of the most commonly diagnosed neoplasms and a leading cause of cancer
death among females worldwide. Limitations with conventional medical treatments have driven researchers to
search for alternative approaches using natural products. This study aimed to detemine potential anti-proliferative
effects of methanol and water extracts of Pyrrosia piloselloides (P. piloselloides) on the HeLa cell line. Methods:
3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assays were performed to determine IC50
concentrations and apoptosis analysis was by flow cytometry. To identify chemical compounds in the extracts, gas
chromatography-mass spectrometry (GC-MS) was employed. Results: P. piloselloides methanol extracts (PPME) showed
antiproliferative effects on HeL awith an IC50 of 16.25μg/mL while the P. piloselloides water extract (PPWE) was without
influence. Neither extract showed any significant effects on apoptosis. GC-MS analysis, revealed 5-hydroxymethylfurfural
(23.1%), allopurinol (8.66%) and 3, 5-dihydroxy-6-methyl-2,3-dihydropyran-4-one (7.41%) as major components in
the PPME, while sulfolan-3-ol (10.1%), linoleic acid (9.06%) and β-sitosterol acetate (7.98%) predominated in the
PPWE case. Conclusion: This first study of P. piloselloides showed PPME to exert potent anti-proliferative effect on
HeLa cell lines. Further research now needs to be performed to establish the mechanisms of inhibition.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods
Analytical techniques for steroid estrogens in water samples - A review

Fang TY, Praveena SM, deBurbure C, Aris AZ, Ismail SN, Rasdi I

Chemosphere, 2016 Dec;165:358-368.
PMID: 27665296 DOI: 10.1016/j.chemosphere.2016.09.051

In recent years, environmental concerns over ultra-trace levels of steroid estrogens concentrations in water samples have increased because of their adverse effects on human and animal life. Special attention to the analytical techniques used to quantify steroid estrogens in water samples is therefore increasingly important. The objective of this review was to present an overview of both instrumental and non-instrumental analytical techniques available for the determination of steroid estrogens in water samples, evidencing their respective potential advantages and limitations using the Need, Approach, Benefit, and Competition (NABC) approach. The analytical techniques highlighted in this review were instrumental and non-instrumental analytical techniques namely gas chromatography mass spectrometry (GC-MS), liquid chromatography mass spectrometry (LC-MS), enzyme-linked immuno sorbent assay (ELISA), radio immuno assay (RIA), yeast estrogen screen (YES) assay, and human breast cancer cell line proliferation (E-screen) assay. The complexity of water samples and their low estrogenic concentrations necessitates the use of highly sensitive instrumental analytical techniques (GC-MS and LC-MS) and non-instrumental analytical techniques (ELISA, RIA, YES assay and E-screen assay) to quantify steroid estrogens. Both instrumental and non-instrumental analytical techniques have their own advantages and limitations. However, the non-instrumental ELISA analytical techniques, thanks to its lower detection limit and simplicity, its rapidity and cost-effectiveness, currently appears to be the most reliable for determining steroid estrogens in water samples.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Fulltext Identification of Antidiabetic Metabolites from Paederia foetida L. Twigs by Gas Chromatography-Mass Spectrometry-Based Metabolomics and Molecular Docking Study

Tan DC, Kassim NK, Ismail IS, Hamid M, Ahamad Bustamam MS

Biomed Res Int, 2019;2019:7603125.
PMID: 31275982 DOI: 10.1155/2019/7603125

Paederia foetida L. (Rubiaceae) is a climber which is widely distributed in Asian countries including Malaysia. The plant is traditionally used to treat various diseases including diabetes. This study is to evaluate the enzymatic inhibition activity of Paederia foetida twigs extracts and to identify the metabolites responsible for the bioactivity by gas chromatography-mass spectrometry (GC-MS) metabolomics profiling. Three different twig extracts, namely, hexane (PFH), chloroform (PFC), and methanol (PFM), were submerged for their α-amylase and α-glucosidase inhibition potential in 5 replicates for each. Results obtained from the loading column scatter plot of orthogonal partial least square (OPLS) model revealed the presence of 12 bioactive compounds, namely, dl-α-tocopherol, n-hexadecanoic acid, 2-hexyl-1-decanol, stigmastanol, 2-nonadecanone, cholest-8(14)-en-3-ol, 4,4-dimethyl-, (3β,5α)-, stigmast-4-en-3-one, stigmasterol, 1-ethyl-1-tetradecyloxy-1-silacyclohexane, ɣ-sitosterol, stigmast-7-en-3-ol, (3β,5α,24S)-, and α-monostearin. In silico molecular docking was carried out using the crystal structure α-amylase (PDB ID: 4W93) and α-glucosidase (PDB ID: 3WY1). α-Amylase-n-hexadecanoic acid exhibited the lowest binding energy of -2.28 kcal/mol with two hydrogen bonds residue, namely, LYS178 and TYR174, along with hydrophobic interactions involving PRO140, TRP134, SER132, ASP135, and LYS172. The binding interactions of α-glucosidase-n-hexadecanoic acid complex ligand also showed the lowest binding energy among 5 major compounds with the energy value of -4.04 kcal/mol. The complex consists of one hydrogen bond interacting residue, ARG437, and hydrophobic interactions with ALA444, ASP141, GLN438, GLU432, GLY374, LEU373, LEU433, LYS352, PRO347, THR445, HIS348, and PRO351. The study provides informative data on the potential antidiabetic inhibitors identified in Paederia foetida twigs, indicating the plant has the therapeutic effect properties to manage diabetes.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Stereoselective method development and validation for determination of concentrations of amphetamine-type stimulants and metabolites in human urine using a simultaneous extraction-chiral derivatization approach

Wan Raihana WA, Gan SH, Tan SC

J Chromatogr B Analyt Technol Biomed Life Sci, 2011 Jan 1;879(1):8-16.
PMID: 21147046 DOI: 10.1016/j.jchromb.2010.10.037

Amphetamine-type stimulants (ATS) are a group of chiral amine drugs which are commonly abused for their sympathomimetic and stimulant properties. ATS are extensively metabolised by hepatic cytochrome P450 enzymes. As metabolism of ATS has been shown to be highly stereospecific, stereoselective analytical methods are essential for the quantitative determination of ATS concentrations for both in vivo and in vitro studies of ATS metabolism. This paper describes a new stereoselective method for the simultaneous determination of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxymethamphetamine (HMMA), 4-hydroxy-3-methoxyamphetamine (HMA), 3,4-hydroxymethamphetamine (HHMA) and 3,4-hydroxyamphetamine (HHA) in human urine samples validated according to the United States Food and Drug Administration guidelines. In this method, analytes are simultaneously extracted and derivatized with R-(-)-α-methoxy-α-(trifluoromethyl)phenylacetyl chloride (R-MTPCl) as the chiral derivatization reagent. Following this, the analytes were subjected to a second derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA) which targets the hydroxyl groups present in HMMA, HMA, HHMA and HHA. The derivatized analytes were separated and quantified using gas chromatography-mass spectrometry (GC-MS). The method was evaluated according to the established guidelines for specificity, linearity, precision, accuracy, recovery and stability using a five-day protocol. Intra-day precision ranged from 0.89 to 11.23% RSD whereas inter-day precision was between 1.03 and 12.95% RSD. Accuracy values for the analytes ranged from -5.29% to 13.75%. Limits of quantitation were 10 μg/L for AM, MA, MDMA, HMA and HMMA and 2μg/L for MDA, HMA and HHA. Recoveries and stability values were also within accepted values. The method was applied to authentic ATS-positive samples.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Fulltext Xanthine Oxidase Inhibitory Activity, Chemical Composition, Antioxidant Properties and GC-MS Analysis of Keladi Candik (Alocasia longiloba Miq)

Abdulhafiz F, Mohammed A, Kayat F, Bhaskar M, Hamzah Z, Podapati SK, et al.

Molecules, 2020 Jun 08;25(11).
PMID: 32521624 DOI: 10.3390/molecules25112658

Alocasia longiloba, locally known as 'Keladi Candik', has been used traditionally to treat wounds, furuncle and joint inflammations. A. longiloba can be a new source of herbal medicine against hyperuricemia by inhibiting the activity of xanthine oxidase enzyme, the enzyme which is responsible for the development of hyperuricemia in human. Existing xanthine oxidase inhibitors (XOI drugs) show several side effects on gout patients. Therefore, an alternative herbal medicine from plants, with high therapeutic property and free of side effects, are greatly needed. This study was conducted to evaluate XO inhibitory activity, chemical composition, antioxidant activity and GC-MS profile of A. longiloba. Our results showed that ethanolic petiole extract exhibited the highest XO inhibitory activity (70.40 ± 0.05%) with IC50 value of 42.71 μg/mL, followed by ethanolic fruit extracts (61.44 ± 1.24%) with the IC50 value of 51.32 μg/mL. In a parallel study, the phytochemical analysis showed the presence of alkaloid, flavonoid, terpenoids, glycoside and saponin in petiole and fruit extracts, as well as higher total phenolic and flavonoid contents and strong scavenging activity on DPPH and ABTS antioxidant assay. The GC-MS analysis of fruit and petiole extracts revealed the presence of various compounds belonging to different chemical nature, among them are limonen-6-ol, α-DGlucopyranoside, paromomycin, aziridine, phenol, Heptatriacotanol, Phen-1,2,3-dimethyl and Betulin found in ethanolic fruit extract, and Phen-1,4-diol,2,3-dimethyl-, 1-Ethynyl-3,trans(1,1-dimethylethyl), Phenol,2,6-dimethoxy-4-(2-propenyl)- and 7-Methyl-Z-tetradecen-1-olacetate found in ethanolic petiole extract. Some compounds were documented as potent anti-inflammatory and arthritis related diseases by other researchers. In this study, the efficiency of solvents to extract bioactives was found to be ethanol > water, methanol > hexane > chloroform. Together, our results suggest the prospective utilization of fruit and petiole of A. longiloba to inhibit the activity of XO enzyme.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry

Zainudin BH, Salleh S, Mohamed R, Yap KC, Muhamad H

Food Chem, 2015 Apr 1;172:585-95.
PMID: 25442595 DOI: 10.1016/j.foodchem.2014.09.123

An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry*
Method development for determination of fluroxypyr in water

Halimah M, Tan YA, Aini K, Ismail BS

J Environ Sci Health B, 2003 Jul;38(4):429-40.
PMID: 12856925

Improved methods for extraction and clean up of fluroxypyr residue in water have been established. Two methods of fluroxypyr extraction were used, namely, Direct Measurement of fluroxypyr and Concentration of fluroxypyr onto A Solid Phase Extraction (SPE) Adsorbent, followed by elution with solvent before determination of fluroxypyr. The recovery for Direct Measurement of fluroxypyr in water containing 8-100 microg L(-1), ranged from 86 to 110% with relative standard deviation of 0.7 to 2.15%. For the second method, three types of SPE were used, viz. C18, C18 end-capped and polyvinyl dibenzene (ISOLUTE ENV+). The procedure involved concentrating the analyte from fluroxypyr-spiked water at pH 3, followed by elution of the analyte with 4 mL of acentonitrile. The recovery of fluroxypyr from the spiked sample at 1 to 50 microg L(-1) after eluting through either C18 or C18 end-capped ranged from 40-64% (with relative standard deviation of 0.7 to 2.15) and 41-65% (with standard deviation of 1.52 to 11.9). The use of ISOLUTE ENV+, gave better results than the C18, C18 end-capped or the Direct Measurement Methods. The recovery and standard deviation of fluroxypyr from spiked water using ISOLUTE ENV+ ranged from 91-102% and 2.5 to 5.3, respectively.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Determination toxic effects of Hystrix Brachyura Bezoar extracts using cancer cell lines and embryo zebrafish (Danio rerio) models and identification of active principles through GC-MS analysis

Firus Khan AY, Ahmed QU, Nippun TS, Hilles A, Jalal TK, Teh LK, et al.

J Ethnopharmacol, 2020 Nov 15;262:113138.
PMID: 32726681 DOI: 10.1016/j.jep.2020.113138

ETHNOPHARMACOLOGICAL RELEVANCE: Porcupine bezoar (PB) is used as folk medicine for various medical conditions including cancer treatment in Malaysia. However, its toxicity profile has never been thoroughly ascertained to confirm its safe nature as an efficacious traditional medicine in the treatment of cancer as well as other ailments.
AIM OF THE STUDY: This study was aimed to reveal three different PBs' aqueous extracts(viz. PB-A, PB-B, PB-C) chemical constituent's profile using GC-MS analysis, anticancer property on A375, HeLa and MCF7 cancer cells, toxicity profile on zebrafish embryo morphology, EC50, LC50 and teratogenicity index.
MATERIALS AND METHODS: PBs' extracts characterization was performed through GC-MS analysis, in vitro anticancer effect was carried out on A375, HeLa and MCF7 cancer cell lines and finally and toxicity properties on three different PBs aqueous extracts (viz. PB-A, PB-B, PB-C) were determined using zebrafish embryo model.
RESULTS: The GC-MS analysis revealed 10 similar compounds in all PBs' extracts. Dilauryl thiodipropionate was found to be a major compound in all PBs' extracts followed by tetradecanoic acid. An in vitro anticancer study revealed PB extracts exerted median inhibition concentration (IC50) <50 μg/mL, on cancer cells viz. A375, HeLa and MCF7 with no significant toxicity on normal cells viz. NHDF cells. In vivo toxicity of PBs extracts found affecting tail detachment, hatching, craniofacial, brain morphology, soft tissues, edema, spinal, somites, notochord and cardiovascular system (brachycardia, disruption of blood circulation) deformities. The LC50 and EC50 demonstrated PB extracts effect as dose and time dependent with median concentration <150.0 μg/mL. Additionally, teratogenicity index (TI) viz. >1.0 revealed teratogenic property for PB extracts.
CONCLUSIONS: The findings revealed that all three PBs aqueous extracts possessed anticancer activity and exhibited significant toxicological effects on zebrafish embryos with high teratogenicity index. Hence, its use as an anticancer agent requires further investigation and medical attentions to determine its safe dose.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Occurrence, distribution, and dechlorination of polychlorinated biphenyls and health risk assessment in Selangor River basin

Sakai N, Dayana E, Abu Bakar A, Yoneda M, Nik Sulaiman NM, Ali Mohd M

Environ Monit Assess, 2016 Oct;188(10):592.
PMID: 27679511

Polychlorinated biphenyls (PCBs) were monitored in surface water collected in the Selangor River basin, Malaysia, to identify the occurrence, distribution, and dechlorination process as well as to assess the potential adverse effects to the Malaysian population. Ten PCB homologs (i.e., mono-CBs to deca-CBs) were quantitated by using gas chromatography-mass spectrometry (GC/MS). The total concentration of PCBs in the 10 sampling sites ranged from limit of detection to 7.67 ng L(-1). The higher chlorinated biphenyls (tetra-CBs to deca-CBs) were almost not detected in most of the sampling sites, whereas lower chlorinated biphenyls (mono-CBs, di-CBs, and tri-CBs) dominated more than 90 % of the 10 homologs in all the sampling sites. Therefore, the PCB load was estimated to be negligible during the sampling period because PCBs have an extremely long half-life. The PCBs, particularly higher chlorinated biphenyls, could be thoroughly dechlorinated to mono-CBs to tri-CBs by microbial decomposition in sediment or could still be accumulated in the sediment. The lower chlorinated biphenyls, however, could be resuspended or desorbed from the sediment because they have faster desorption rates and higher solubility, compared to the higher chlorinated biphenyls. The health risk for the Malaysia population by PCB intake that was estimated from the local fish consumption (7.2 ng kg(-1) bw day(-1)) and tap water consumption (1.5 × 10(-3)-3.1 × 10(-3) ng kg(-1) bw day(-1)) based on the detected PCB levels in the surface water was considered to be minimal. The hazard quotient based on the tolerable daily intake (20 ng kg(-1) bw day(-1)) was estimated at 0.36.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods
Fulltext Biological activity of carbazole alkaloids and essential oil of Murraya koenigii against antibiotic resistant microbes and cancer cell lines

Nagappan T, Ramasamy P, Wahid ME, Segaran TC, Vairappan CS

Molecules, 2011 Nov 21;16(11):9651-64.
PMID: 22105714 DOI: 10.3390/molecules16119651

A total of three carbazole alkaloids and essential oil from the leaves of Murraya koenigii (Rutaceae) were obtained and examined for their effects on the growth of five antibiotic resistant pathogenic bacteria and three tumor cell lines (MCF-7, P 388 and Hela). The structures of these carbazoles were elucidated based on spectroscopy data and compared with literature data, hence, were identified as mahanine (1), mahanimbicine (2) and mahanimbine (3). The chemical constituents of the essential oil were identified using Gas Chromatography-Mass Spectroscopy (GCMS). These compounds exhibited potent inhibition against antibiotic resistant bacteria such as Staphylococcus aureus (210P JTU), Psedomonas aeruginosa (ATCC 25619), Klebsiella pneumonia (SR1-TU), Escherchia coli (NI23 JTU) and Streptococcus pneumoniae (SR16677-PRSP) with significant minimum inhibition concentration (MIC) values (25.0-175.0 mg/mL) and minimum bacteriacidal concentrations (MBC) (100.0-500.0 mg/mL). The isolated compounds showed significant antitumor activity against MCF-7, Hela and P388 cell lines. Mahanimbine (3) and essential oil in particular showed potent antibacteria and cytotoxic effect with dose dependent trends (≤5.0 μg/mL). The findings from this investigation are the first report of carbazole alkaloids' potential against antibiotic resistant clinical bacteria, MCF-7 and P388 cell lines.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods
Fulltext Evaluation of Antioxidative and Cytotoxic Activities of Streptomyces pluripotens MUSC 137 Isolated from Mangrove Soil in Malaysia

Ser HL, Ab Mutalib NS, Yin WF, Chan KG, Goh BH, Lee LH

Front Microbiol, 2015;6:1398.
PMID: 26733951 DOI: 10.3389/fmicb.2015.01398

Streptomyces pluripotens MUSC 137 was isolated from mangrove soil obtained from Tanjung Lumpur, Pahang, Malaysia. We investigated the phylogenetic, genomic, biochemical, and phenotypic characteristics of this strain. Uniquely adapted microorganisms from mangrove habitats have previously yielded compounds of biopharmaceutical interest. In order to examine the bioactivities possessed by the strain, fermentation extract was prepared through solvent extraction method prior to bioactivities screenings. Antioxidant activity was examined via DPPH assay while the cytotoxic effect was assessed by means of examining the activity of the extract against selected human cancer cell lines, namely colon cancer cells (HCT-116, Caco-2, SW480, and HT-29), breast cancer cell (MCF-7), lung cancer cell (A549), prostate cancer cell (DU145), and cervical cancer cell (Ca Ski). The results revealed MUSC 137 possesses significant antioxidant activity and demonstrates cytotoxic effect against several cancer cell lines tested. The results indicated MCF-7 cells were most susceptible to the extract with the lowest IC50 (61.33 ± 17.10 μg/mL), followed by HCT-116 and A549. Additionally, selective index (SI) showed that MUSC 137 extract was less toxic against normal cell lines when compared to MCF-7 and HCT-116 cells. The extract was further subjected to chemical analysis using GC-MS and revealed the presence of deferoxamine and pyrrolizidines related compounds which may account for the antioxidant and cytotoxic properties observed.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Catalytic thermolysis in treating Cibacron Blue in aqueous solution: Kinetics and degradation pathway

Su CX, Teng TT, Wong YS, Morad N, Rafatullah M

Chemosphere, 2016 Mar;146:503-10.
PMID: 26741557 DOI: 10.1016/j.chemosphere.2015.12.048

A thermal degradation pathway of the decolourisation of Reactive Cibacron Blue F3GA (RCB) in aqueous solution through catalytic thermolysis is established. Catalytic thermolysis is suitable for the removal of dyes from wastewater as it breaks down the complex dye molecules instead of only transferring them into another phase. RCB is a reactive dye that consists of three main groups, namely anthraquinone, benzene and triazine groups. Through catalytic thermolysis, the bonds that hold the three groups together were effectively broken and at the same time, the complex molecules degraded to form simple molecules of lower molecular weight. The degradation pathway and products were characterized and determined through UV-Vis, FT-IR and GCMS analysis. RCB dye molecule was successfully broken down into simpler molecules, namely, benzene derivatives, amines and triazine. The addition of copper sulphate, CuSO4, as a catalyst, hastens the thermal degradation of RCB by aiding in the breakdown of large, complex molecules. At pH 2 and catalyst mass loading of 5 g/L, an optimum colour removal of 66.14% was observed. The degradation rate of RCB is well explained by first order kinetics model.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Advanced analytical techniques for the extraction and characterization of plant-derived essential oils by gas chromatography with mass spectrometry

Waseem R, Low KH

J Sep Sci, 2015 Feb;38(3):483-501.
PMID: 25403494 DOI: 10.1002/jssc.201400724

In recent years, essential oils have received a growing interest because of the positive health effects of their novel characteristics such as antibacterial, antifungal, and antioxidant activities. For the extraction of plant-derived essential oils, there is the need of advanced analytical techniques and innovative methodologies. An exhaustive study of hydrodistillation, supercritical fluid extraction, ultrasound- and microwave-assisted extraction, solid-phase microextraction, pressurized liquid extraction, pressurized hot water extraction, liquid-liquid extraction, liquid-phase microextraction, matrix solid-phase dispersion, and gas chromatography (one- and two-dimensional) hyphenated with mass spectrometry for the extraction through various plant species and analysis of essential oils has been provided in this review. Essential oils are composed of mainly terpenes and terpenoids with low-molecular-weight aromatic and aliphatic constituents that are particularly important for public health.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Utilization of palm oil sludge through pyrolysis for bio-oil and bio-char production

Thangalazhy-Gopakumar S, Al-Nadheri WM, Jegarajan D, Sahu JN, Mubarak NM, Nizamuddin S

Bioresour Technol, 2015 Feb;178:65-9.
PMID: 25278112 DOI: 10.1016/j.biortech.2014.09.068

In this study, pyrolysis technique was utilized for converting palm oil sludge to value added materials: bio-oil (liquid fuel) and bio-char (soil amendment). The bio-oil yield obtained was 27.4±1.7 wt.% having a heating value of 22.2±3.7 MJ/kg and a negligible ash content of 0.23±0.01 wt.%. The pH of bio-oil was in alkaline region. The bio-char yielded 49.9±0.3 wt.%, which was further investigated for sorption efficiency by adsorbing metal (Cd(2+) ions) from water. The removal efficiency of Cd(2+) was 89.4±2%, which was almost similar to the removal efficiency of a commercial activated carbon. The adsorption isotherm was well described by Langmuir model. Therefore, pyrolysis is proved as an efficient tool for palm oil sludge management, where the waste was converted into valuable products.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry

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