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Occurrence, distribution, and ecological risk of bisphenol analogues in marine ecosystem of urbanized coast and estuary

Zainuddin AH, Roslan MQJ, Razak MR, Yusoff FM, Haron DEM, Aris AZ

Mar Pollut Bull, 2023 Jul;192:115019.
PMID: 37201347 DOI: 10.1016/j.marpolbul.2023.115019

Bisphenol analogues are prevalent globally because of rampant usage and imprecise processing techniques, prompting alerts about environmental and health hazards. The method employed in this study by solid phase extraction (SPE) and liquid chromatography-tandem quadrupole mass spectrometer (LC-MS/MS) for both quantification and qualitative analysis of the bisphenol compounds in the surface water samples. The coastal and estuarine surface water of Port Dickson and Lukut ranges from 1.32 ng/L to 1890.51 ng/L of bisphenol analogues. BPF mean concentration at 1143.88 ng/L is the highest, followed by BPA and BPS at 59.01 ng/L and 10.96 ng/L, respectively. Based on RQm for bisphenol analogues, the highest for BPF at 2.49 (RQ > 1, high risk), followed by BPS at 0.12 (0.1

Matched MeSH terms: Chromatography, Liquid
Fulltext Urinary aluminium and its association with autism spectrum disorder in urban preschool children in Malaysia

Abd Wahil MS, Ja'afar MH, Md Isa Z

PeerJ, 2023;11:e15132.
PMID: 37197586 DOI: 10.7717/peerj.15132

BACKGROUND: The presence of aluminium (Al) in the human body may impact brain neurodevelopment and function, and it is thought to contribute to autism spectrum disease (ASD). The main objective of this study was to assess the association between urinary Al and the development of ASD among Malaysian preschool children in the urban city of Kuala Lumpur.
METHOD: This was an unmatched case-control study in which children with ASD were recruited from an autism early intervention center and typically developed (TD) children were recruited from government-run nurseries and preschools. Urine samples were collected at home, assembled temporarily at study locations, and transported to the laboratory within 24 h. The Al concentration in the children's urine samples was determined using inductively coupled plasma mass spectrometry (ICP-MS).
RESULT: A total of 155 preschool children; 81 ASD children and 74 TD children, aged 3 to 6 years, were enlisted in the study. This study demonstrated that ASD children had significantly higher urinary Al levels than TD children (median (interquartile range (IQR): 2.89 (6.77) µg/dL versus 0.96 (2.95) µg/dL) (p 1, p

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
The antioxidant and antimicrobial activity of ethanolic extract in roots, stems, and leaves of three commercial Cymbopogon species

Wahyuni DK, Kharisma VD, Murtadlo AAA, Rahmawati CT, Syukriya AJ, Prasongsuk S, et al.

BMC Complement Med Ther, 2024 Jul 18;24(1):272.
PMID: 39026301 DOI: 10.1186/s12906-024-04573-4

BACKGROUND: Cymbopogon is a member of the family Poaceae and has been explored for its phytochemicals and bioactivities. Although the antimicrobial activities of Cymbopogon spp. extracts have been extensively studied, comprehensive analyses are required to identify promising compounds for the treatment of antimicrobial resistance. Therefore, this study investigated the antioxidant and antimicrobial properties of Cymbopogon spp. ethanolic extracts in every single organ.
METHODS: Ethanolic extracts were obtained from three Indonesian commercial species of Cymbopogon spp., namely Cymbopogon citratus (L.) Rendle, Cymbopogon nardus (DC.) Spatf., and Cymbopogon winterianus Jowitt. The leaf, stem, and root extracts were evaluated via metabolite profiling using gas chromatography-mass spectrometry (GC-MS). In silico and in vitro analyses were used to evaluate the antioxidant and antimicrobial properties of the Cymbopogon spp. ethanolic extracts. In addition, bioactivity was measured using cytotoxicity assays. Antioxidant assays were performed using 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2-azino-bis [3-ethylbenzothiazoline-6-sulfonic acid (ABTS) to determine toxicity to Huh7it-1 cells using a tetrazolium bromide (MTT) assay. Finally, the antimicrobial activity of these extracts was evaluated against Candida albicans, Bacillus subtilis, Staphylococcus aureus, and Escherichia coli using a well diffusion assay.
RESULTS: GC-MS analysis revealed 53 metabolites. Of these, 2,5-bis(1,1-dimethylethyl)- phenol (27.87%), alpha-cadinol (26.76%), and 1,2-dimethoxy-4-(1-propenyl)-benzene (20.56%) were the predominant compounds. C. winterianus and C. nardus leaves exhibited the highest antioxidant activity against DPPH and ABTS, respectively. Contrastingly, the MTT assay showed low cytotoxicity. C. nardus leaf extract exhibited the highest antimicrobial activity against E. coli and S. aureus, whereas C. winterianus stem extract showed the highest activity against B. substilis. Furthermore, computational pathway analysis predicted that antimicrobial activity mechanisms were related to antioxidant activity.
CONCLUSIONS: These findings demonstrate that the leaves had strong antioxidant activity, whereas both the leaves and stems showed great antimicrobial activity. Furthermore, all Cymbopogon spp. ethanolic extracts showed low toxicity. These findings provide a foundation for future studies that assess the clinical safety of Cymbopogon spp. as novel drug candidates.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
High performance liquid chromatography (HPLC) method for confirming thin layer chromatography (TLC) findings in inborn errors of metabolism children in Malaysia

Yahya NA, Ismail Z, Embong KH, Mohamad SA

Southeast Asian J Trop Med Public Health, 1995;26 Suppl 1:130-3.
PMID: 8629091

High performance liquid chromatography (HPLC) with phenylisothiocyanate (PITC) is recently used for confirming the diagnosis of inborn errors of metabolism (IEM) especially amino acid disorders in Malaysian children. The method of HPLC used is a precolumn derivatization of amino acids with phenylisothiocyanate and is separated by reversed phase chromatography using 3.9 x 300 mm free amino acid columns and is detected by a UV/Vis detector. The samples are obtained from cases suspected of inborn errors of metabolism, especially of amino acid disorders, which are detected clinically by pediatricians. Initially, samples from patients suspected of inborn errors of metabolism, either urine or serum, are run on one-dimensional thin layer chromatography and supplementary chemical tests to detect the abnormal bands and associated abnormalities respectively. Positive samples are further run on HPLC to determine the specific amino acids abnormality. An examples of a case of maple syrup urine disease is discussed, based on the thin layer chromatography findings and HPLC findings.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods; Chromatography, Thin Layer/methods
Preliminary studies on the effect of excretory secretory (ES) Ascaris lumbricoides antigens on colorectal cell line viability

Ab Talib NN, Nisha M, Ramasamy R, Pang JC

Trop Biomed, 2024 Jun 01;41(2):160-165.
PMID: 39154268 DOI: 10.47665/tb.41.2.005

Helminth parasites are a group of complex metazoans from various taxonomic families. Excretory secretory (ES) by-products, secreted by living parasites from the surface, appeared to modulate the host immunological response towards helminth infection. This study aims to investigate the effect of ES antigen from helminth parasite on colorectal cell viability. Worm were cultured in phosphate-buffered saline (PBS x1) at 37°C for 24 hours after being rinsed in sterile PBS. Using a mortar and pestle, the worm was crushed vigorously using PBS. The obtained excretory secretory (ES) antigens were extracted and filtered using a 0.22 µM filter and stored at -20°C for further assay. For LCMS, 100 µl of the extract was analysed using Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HT. The extraction of ES antigen (10 µg/ml and 20 µg/ml) was used for cell viability studies using CRC cell line HCT 116. Cell viability and MTT assay were conducted as per the protocol mentioned in the MTT kit. The liquid chromatography and mass spectrometry (LCMS) data indicated that the ES antigen contained metabolic compounds, namely fatty acid, amino alcohol, indoles, sterols, glycosides, and sphingoids. For the Ascaris lumbricoides LCMS analyses, around 405 metabolic peaks were detected. Out of which, 58 were detected via the database were identified, while several compounds detected have anticancer properties. The MTT assay indicated that after 24 hours and 48 hours of exposure, all treated cells showed a decrease in cell viability compared to the control group. The preliminary studies demonstrated that the ES antigen from Ascaris lumbricoides has some ability to decrease the cell viability of the HCT116 CRC cell line. Further studies are needed to examine the cell cycle arrest and apoptosis effect of the ES antigen towards the CRC cell line.

Matched MeSH terms: Chromatography, Liquid
Metabolite profiling from different parts of tender fruit endosperm of Borassus flabellifer L. (ice apple)

Vasudevan V, Prabaharan J, Krishnan N, K A, Gopinath SCB, Raman P

Anal Methods, 2023 Aug 03;15(30):3735-3751.
PMID: 37493014 DOI: 10.1039/d3ay00704a

Borassus flabellifer L., commonly known as Asian palmyra, is native to South and Southeast Asia. The endosperms of B. flabellifer (known as nungu in Dravidian culture) are widely consumed during the summer season. It is rich in various nutrients and helps in reducing weight, treating skin and digestive issues, lowering body temperature, and managing migraines and diabetes. This study focuses on identifying the small molecules and proteins from the two varieties of B. flabellifer tender fruit endosperms collected from districts around Chennai, Tamil Nadu, India. The collected free nuclear endosperm was subjected to direct extraction and the mesocarp and cellular endosperms were lyophilized and homogenized. Metabolites were extracted by hexane, methanol, and chloroform and investigated using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). The compounds identified were from the classes of carboxylic acids, flavonoids, amino acids, alkaloids, fatty acids, oligopeptides, vitamins, and glycosides. High-performance liquid chromatography (HPLC) technique was employed to estimate the quantity of amino acids, wherein the total amino acid in the green variety was found to be higher than in the black variety. Proteins were identified after simulating with a gastrointestinal enzyme using liquid chromatography tandem mass spectrometry (LC-MS/MS)-based peptide mass fingerprinting. The different mineral oxides present in the tender fruit endosperm were identified using X-ray diffraction studies, which confirmed the presence of mineral oxides, such as Br1.25ClO2.75Pb3.88, calcium zirconium tantalum oxide, and barium fluoroniobate. This study validates the presence of bioactive metabolites in green and black varieties of B. flabellifer tender fruit endosperm with a range of activities, such as anti-inflammatory, antibacterial, anticancer, and anti-diabetic properties.

Matched MeSH terms: Chromatography, Liquid
Fulltext Antimicrobial Potential of Aqueous Extract of Giant Sword Fern and Ultra-High-Performance Liquid Chromatography-High-Resolution Mass Spectrometry Analysis

Venmathi Maran BA, Palaniveloo K, Mahendran T, Chellappan DK, Tan JK, Yong YS, et al.

Molecules, 2023 Aug 15;28(16).
PMID: 37630329 DOI: 10.3390/molecules28166075

Vibriosis and parasitic leech infestations cause the death of various farmed fish, such as groupers, hybrid groupers, sea bass, etc., in Malaysia and other Southeast Asian countries. In the absence of natural control agents, aquaculture operators rely on toxic chemicals to control Vibrio infections and parasitic leeches, which can have a negative impact on the environment and health. In the present study, we investigated the antivibrio and antiparasitic activities of the aqueous extract of giant sword fern (GSF) (Nephrolepis biserrata, Nephrolepidaceae, locally known as "Paku Pedang") against four Vibrio spp. and the parasitic leech Zeylanicobdella arugamensis, as well as its metabolic composition using the ultra-high-performance liquid chromatography-high-resolution mass spectrometry system (UHPLC-HRMS). The data show that the aqueous extract of GSF at a concentration of 100 mg/mL exhibits potent bactericidal activity against V. parahaemolyticus with a zone of inhibition of 19.5 mm. In addition, the extract showed dose-dependent activity against leeches, resulting in the complete killing of the parasitic leeches within a short period of 11-43 min when tested at concentrations ranging from 100 to 25 mg/mL. The UHPLC-HRMS analysis detected 118 metabolites in the aqueous extract of GSF. Flavonoids were the primary metabolites, followed by phenolic, aromatic, fatty acyl, terpenoid, vitamin and steroidal compounds. Notably, several of these metabolites possess antibacterial and antiparasitic properties, including cinnamaldehyde, cinnamic acid, apigenin, quercetin, cynaroside, luteolin, naringenin, wogonin, 6-gingerol, nicotinamide, abscisic acid, daidzein, salvianolic acid B, etc. Overall, our study shows the significant antibacterial and antiparasitic potential of the GSF aqueous extract, which demonstrates the presence of valuable secondary metabolites. Consequently, the aqueous extract is a promising natural alternative for the effective control of Vibrio infections and the treatment of parasitic leeches in aquaculture systems.

Matched MeSH terms: Chromatography, High Pressure Liquid
Fulltext Evaluation of bioactive compounds from Ficus carica L. leaf extracts via high-performance thin-layer chromatography combined with effect-directed analysis

Agatonovic-Kustrin S, Wong S, Dolzhenko AV, Gegechkori V, Ku H, Tucci J, et al.

J Chromatogr A, 2023 Sep 13;1706:464241.
PMID: 37541060 DOI: 10.1016/j.chroma.2023.464241

This study compares different solvent systems with the use of spontaneous fermentation on the phytochemical composition of leaf extracts from a locally grown white variety of common fig (Ficus carica Linn.). The aim was to detect and identify bioactive compounds that are responsible for acetylcholinesterase (AChE), α-amylase and cyclooxygenase-1 (COX-1) enzyme inhibition, and compounds that exhibit antimicrobial activity. Bioactive zones in chromatograms were detected by combining High-performance thin-layer chromatography (HPTLC) with enzymatic and biological assays. A new experimental protocol for measuring the relative half-maximum inhibitory concentration (IC50) was designed to evaluate the potency of the extracts compared to the potency of known inhibitors. Although the IC50 of the fig leaf extract for α-amylase and AChE inhibition were significantly higher when compared to IC50 for acarbose and donepezil, the COX-1 inhibition by the extract (IC50 = 627 µg) was comparable to that of salicylic acid (IC50 = 557 µg), and antimicrobial activity of the extract (IC50 = 375-511 µg) was similar to ampicillin (IC50 = 495 µg). Four chromatographic zones exhibited bioactivity. Compounds from detected bioactive bands were provisionally identified by comparing the band positions to coeluted standards, and by Fourier transform infrared (FTIR) spectra from eluted zones. Flash chromatography was used to separate selected extract into fractions and isolate fractions that are rich in bioactive compounds for further characterisation with nuclear magnetic resonance (NMR) spectroscopy and liquid chromatography-mass spectrometry (LC-MS) analysis. The main constituents identified were umbelliferon (zone 1), furocoumarins psoralen and bergapten (zone 2), different fatty acids (zone 3 and 4), and pentacyclic triterpenoids (calotropenyl acetate or lupeol) and stigmasterol (zone 4).

Matched MeSH terms: Chromatography, Thin Layer
Separation of Antioxidant-Rich Alternanthera Sessilis Red Extracts by Sephadex LH-20 and Identification of Polyphenols Using HPLC-QToF-MS/MS

Hwong CS, Leong KH, Aziz AA, Kong KW

Chem Biodivers, 2023 Jul;20(7):e202300215.
PMID: 37278124 DOI: 10.1002/cbdv.202300215

This study aimed to fractionate Alternanthera sessilis Red (ASR) crude extracts and determine their antioxidant activities as well as the related active components in the whole plant. ASR was extracted with water and ethanol, and further separated using a Sephadex LH-20 column. Following the assessments of the polyphenolic contents and antioxidant activities of crude extracts (H2 OASR and EtOHASR ) and fractions, a HPLC-QToF analysis was performed on the crude extracts and selected fractions (H2 OASR FII and EtOHASR FII). Three water fractions (H2 OASR FI, FII and FIII) and four ethanolic fractions (EtOHASR FI, FII, FIII and FIV) were derived from their crude extracts, respectively. EtOHASR FII exhibited the greatest total phenolic content (120.41 mg GAE/g fraction), total flavonoid content (223.07 mg RE/g fraction), and antioxidant activities (DPPH IC50 =159.43 μg/mL; FRAP=1.93 mmol Fe2+ /g fraction; TEAC=0.90 mmol TE/g fraction). Correlation analysis showed significant (p<0.01) positive correlations between both TPC (r=0.748-0.970) and TFC (r=0.686-0.949) with antioxidant activities in the crude extracts and fractions. Flavonoids were the major compounds in the four selected samples tentatively identified using HPLC-QToF-MS/MS, with the highest number of 30 polyphenol compounds detected in the most active fraction, EtOHASR FII.

Matched MeSH terms: Chromatography, High Pressure Liquid
A Limited Survey of Aflatoxins and Zearalenone in Feed and Feed Ingredients from Pakistan

Iqbal SZ, Asi MR, Nisar S, Zia KM, Jinap S, Malik N

J Food Prot, 2016 Oct;79(10):1798-1801.
PMID: 28221839 DOI: 10.4315/0362-028X.JFP-16-091

This work presents current information on the presence of aflatoxins (AFs) and zearalenone (ZEN) in feed and feed ingredients from Punjab, Pakistan. The 105 samples tested were concentrated feed, i.e., cotton seed meal (18 samples) and soybean meal (14), and feed ingredients, i.e., crushed corn (17), crushed wheat (15), barley (17). and poultry feed (24). Samples were analyzed using high-performance liquid chromatography equipped with a fluorescence detector. Analysis revealed that 69 of 105 samples were contaminated with AFs, and the highest mean concentrations of AFB1 (6.20 μg/kg) and total AFs (9.30 μg/kg) were found in poultry feed samples. The mean total AF concentrations ranged from the limit of quantification to 165.5 μg/kg. However, 75 of the 105 samples were positive for ZEN. The highest mean concentration (19.45 μg/kg) was found in poultry feed samples. The mean ZEN concentrations were 0.15 to 145.30 μg/kg. The prevalence of AFs and ZEN was high in feed and feed ingredients and needs urgent attention.

Matched MeSH terms: Chromatography, High Pressure Liquid
Essential oils composition of Litsea glauca and Litsea fulva and their anticholinesterase inhibitory activity

Salleh WMNHW, Salihu AS, Ab Ghani N

Nat Prod Res, 2024;38(4):629-633.
PMID: 36794425 DOI: 10.1080/14786419.2023.2180507

This study was designed to examine the essential oils compositions of Litsea glauca Siebold and Litsea fulva Fern.-Vill. growing in Malaysia. The essential oils were achieved by hydrodistillation and fully characterized by gas chromatography (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The study identified 17 and 19 components from the leaf oils from L. glauca (80.7%) and L. fulva (81.5%), respectively. The major components of L. glauca oil were β-selinene (30.8%), β-calacorene (11.3%), tridecanal (7.6%), isophytol (4.8%) and β-eudesmol (4.5%); whereas in L. fulva oil gave β-caryophyllene (27.8%), caryophyllene oxide (12.8%), α-cadinol (6.3%), (E)-nerolidol (5.7%), β-selinene (5.5%) and tridecanal (5.0%). Anticholinesterase activity was evaluated using Ellman method. The essential oils showed moderate inhibitory activity on acetylcholinesterase and butyrylcholinesterase assays. Our findings demonstrate that the essential oil could be very useful for the characterization, pharmaceutical, and therapeutic applications of the essential oil from the genus Litsea.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
The occurrence and probabilistic risk of exposure to parabens from bottled and hand-shaken teas in the general adult population of Taiwan

Chin WS, Chang CH, Say YH, Chuang YN, Wang JN, Kao HC, et al.

Environ Sci Pollut Res Int, 2024 Jan;31(3):4518-4527.
PMID: 38102436 DOI: 10.1007/s11356-023-31348-0

Parabens (PBs) are esters of p-hydroxybenzoic acid, and there are growing concerns due to their potential to disrupt endocrine function and their wide use as preservatives in foodstuffs, including beverages. The consumption of bottled and hand-shaken teas is gradually replacing traditional tea consumption through brewing. However, no study has reported PB concentrations in different types of teas or packaging and their associated health risks. Our aim was to determine the concentration of PBs (methyl- (MetPB), ethyl- (EthPB), propyl- (PropPB), butyl-paraben (ButPB)) in green, black, and oolong teas in two varieties of products (bottled and hand-shaken teas), using UPLC-MS/MS. Additionally, we estimated the health risks associated with tea consumption in the general adult population of Taiwan. A Monte Carlo simulation was applied to estimate the distribution of daily PB intake through bottled (n = 79) and hand-shaken (n = 71) tea consumption. Our findings revealed geometric mean concentrations in bottled green/black/oolong teas were 714.1/631.2/532.1 ng/L for MetPB, 95.2/ 30.5/14.9 ng/L for EthPB, 77.9/28.3/non-detected (ND) ng/L for PropPB, and 69.3/26.6/ND ng/L for ButPB. Hand-shaken green/black/oolong teas exhibited concentrations of 867.5/2258/1307 ng/L for MetPB, 28.5/28.8/14.5 ng/L for EthPB, 25.4/18.3/17.8 ng/L for PropPB, and 30.3/18.0/15.5 ng/L for ButPB. The median MetPB concentrations in hand-shaken black (2333 ng/L) and oolong teas (1215 ng/L) were significantly higher than those in bottled black (595.4 ng/L) and oolong teas (489.3 ng/L). Conversely, median concentrations of EthPB, PropPB, and ButPB in bottled teas were significantly higher than those in hand-shaken teas. MetPB was the predominant PB, constituting 73.2-91.9% in bottled teas and 85-94% in hand-shaken teas. Our results showed no health risks associated with bottled or hand-shaken tea consumption based on reference doses. However, the study highlights the importance of continued vigilance given the potential chronic exposure to PBs from various sources, necessitating ongoing concern despite the absence of immediate risks from tea consumption.

Matched MeSH terms: Chromatography, Liquid
Development and validation of a selective, sensitive and stability indicating UPLC-MS/MS method for rapid, simultaneous determination of six process related impurities in darunavir drug substance

A VBR, Yusop Z, Jaafar J, Aris AB, Majid ZA, Umar K, et al.

J Pharm Biomed Anal, 2016 Sep 05;128:141-148.
PMID: 27262107 DOI: 10.1016/j.jpba.2016.05.026

In this study a sensitive and selective gradient reverse phase UPLC-MS/MS method was developed for the simultaneous determination of six process related impurities viz., Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V and Imp-VI in darunavir. The chromatographic separation was performed on Acquity UPLC BEH C18 (50 mm×2.1mm, 1.7μm) column using gradient elution of acetonitrile-methanol (80:20, v/v) and 5.0mM ammonium acetate containing 0.01% formic acid at a flow rate of 0.4mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously using multiple reaction monitoring (MRM) for the quantification of all six impurities in darunavir. The developed method was fully validated following ICH guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness and sample solution stability. The method was able to quantitate Imp-I, Imp-IV, Imp-V at 0.3ppm and Imp-II, Imp-III, and Imp-VI at 0.2ppm with respect to 5.0mg/mL of darunavir. The calibration curves showed good linearity over the concentration range of LOQ to 250% for all six impurities. The correlation coefficient obtained was >0.9989 in all the cases. The accuracy of the method lies between 89.90% and 104.60% for all six impurities. Finally, the method has been successfully applied for three formulation batches of darunavir to determine the above mentioned impurities, however no impurity was found beyond the LOQ. This method is a good quality control tool for the trace level quantification of six process related impurities in darunavir during its synthesis.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Chemometric approach to the optimization of HS-SPME/GC-MS for the determination of multiclass pesticide residues in fruits and vegetables

Abdulra'uf LB, Tan GH

Food Chem, 2015 Jun 15;177:267-73.
PMID: 25660885 DOI: 10.1016/j.foodchem.2015.01.031

An HS-SPME method was developed using multivariate experimental designs, which was conducted in two stages. The significance of each factor was estimated using the Plackett-Burman (P-B) design, for the identification of significant factors, followed by the optimization of the significant factors using central composite design (CCD). The multivariate experiment involved the use of Minitab® statistical software for the generation of a 2(7-4) P-B design and CCD matrices. The method performance evaluated with internal standard calibration method produced good analytical figures of merit with linearity ranging from 1 to 500 μg/kg with correlation coefficient greater than 0.99, LOD and LOQ were found between 0.35 and 8.33 μg/kg and 1.15 and 27.76 μg/kg respectively. The average recovery was between 73% and 118% with relative standard deviation (RSD=1.5-14%) for all the investigated pesticides. The multivariate method helps to reduce optimization time and improve analytical throughput.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Assessment of dispersive liquid-liquid microextraction conditions for gas chromatography time-of-flight mass spectrometry identification of organic compounds in honey

Moniruzzaman M, Rodríguez I, Rodríguez-Cabo T, Cela R, Sulaiman SA, Gan SH

J Chromatogr A, 2014 Nov 14;1368:26-36.
PMID: 25441341 DOI: 10.1016/j.chroma.2014.09.057

The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Fulltext Rapid and simultaneous quantification of levetiracetam and its carboxylic metabolite in human plasma by liquid chromatography tandem mass spectrometry

Yeap LL, Lo YL

PLoS One, 2014;9(11):e111544.
PMID: 25375249 DOI: 10.1371/journal.pone.0111544

A simple liquid chromatography tandem mass spectrometry method was developed and validated according to the guidelines of the US Food and Drug Administration and the European Medicines Agency for a simultaneous quantification of levetiracetam (LEV) and its metabolite, UCB L057 in the plasma of patients. A 0.050 mL plasma sample was prepared by a simple and direct protein precipitation with 0.450 mL acetonitrile (ACN) containing 1 µg/mL of internal standard (IS, diphenhydramine), then vortex mixed and centrifuged. A 0.100 mL of the clear supernatant was diluted with 0.400 mL water and well mixed. A 0.010 mL of the resultant solution was injected into an Agilent Zorbax SB-C18 (2.1 mm×100 mm, 3.5 µm) column with an isocratic elution at 0.5 mL/min using a mixture of 0.1% formic acid in water and ACN (40:60 v/v). Detection was performed using an AB Sciex API 3000 triple quadrupole mass spectrometer, equipped with a Turbo Ion Spray source, operating in a positive mode: LEV at transition 171.1>154.1, UCB L057 at 172.5>126.1, and IS at 256.3>167.3; with an assay run time of 2 minutes. The lower limit of quantification (LLOQ) for both LEV and UCB L057 was validated at 0.5 µg/mL, while their lower limit of detection (LOD) was 0.25 µg/mL. The calibration curves were linear between 0.5 and 100 µg/mL for both analytes. The inaccuracy and imprecision of both intra-assay and inter-assay were less than 10%. Matrix effects were consistent between sources of plasma and the recoveries of all compounds were between 100% and 110%. Stability was established under various storage and processing conditions. The carryovers from both LEV and UCB L057 were less than 6% of the LLOQ and 0.13% of the IS. This assay method has been successfully applied to a population pharmacokinetic study of LEV in patients with epilepsy.

Matched MeSH terms: Chromatography, Liquid*
Novel lipase purification methods - a review of the latest developments

Tan CH, Show PL, Ooi CW, Ng EP, Lan JC, Ling TC

Biotechnol J, 2015 Jan;10(1):31-44.
PMID: 25273633 DOI: 10.1002/biot.201400301

Microbial lipases are popular biocatalysts due to their ability to catalyse diverse reactions such as hydrolysis, esterification, and acidolysis. Lipases function efficiently on various substrates in aqueous and non-aqueous media. Lipases are chemo-, regio-, and enantio-specific, and are useful in various industries, including those manufacturing food, detergents, and pharmaceuticals. A large number of lipases from fungal and bacterial sources have been isolated and purified to homogeneity. This success is attributed to the development of both conventional and novel purification techniques. This review highlights the use of these techniques in lipase purification, including conventional techniques such as: (i) ammonium sulphate fractionation; (ii) ion-exchange; (iii) gel filtration and affinity chromatography; as well as novel techniques such as (iv) reverse micellar system; (v) membrane processes; (vi) immunopurification; (vi) aqueous two-phase system; and (vii) aqueous two-phase floatation. A summary of the purification schemes for various bacterial and fungal lipases are also provided.

Matched MeSH terms: Chromatography/methods*
Co-solvent selection for supercritical fluid extraction of astaxanthin and other carotenoids from Penaeus monodon waste

Radzali SA, Baharin BS, Othman R, Markom M, Rahman RA

J Oleo Sci, 2014;63(8):769-77.
PMID: 25007745

In recent years, astaxanthin is claimed to have a 10 times higher antioxidant activity than that of other carotenoids such as lutein, zeaxanthin, canthaxanthin, and β-carotene; the antioxidant activity of astaxanthin is 100 times higher than that of α-tocopherol. Penaeus monodon (tiger shrimp) is the largest commercially available shrimp species and its waste is a rich source of carotenoids such as astaxanthin and its esters. The efficient and environment-friendly recovery of astaxanthins was accomplished by using a supercritical fluid extraction (SFE) technique. The effects of different co-solvents and their concentrations on the yield and composition of the extract were investigated. The following co-solvents were studied prior to the optimization of the SFE technique: ethanol, water, methanol, 50% (v/v) ethanol in water, 50% (v/v) methanol in water, 70% (v/v) ethanol in water, and 70% (v/v) methanol in water. The ethanol extract produced the highest carotenoid yield (84.02 ± 0.8 μg/g) dry weight (DW) with 97.1% recovery. The ethanol extract also produced the highest amount of the extracted astaxanthin complex (58.03 ± 0.1 μg/g DW) and the free astaxanthin content (12.25 ± 0.9 μg/g DW) in the extract. Lutein and β-carotene were the other carotenoids identified. Therefore, ethanol was chosen for further optimization studies.

Matched MeSH terms: Chromatography, Supercritical Fluid/methods*
Fulltext Antimicrobial compounds from leaf extracts of Jatropha curcas, Psidium guajava, and Andrographis paniculata

Rahman MM, Ahmad SH, Mohamed MT, Ab Rahman MZ

ScientificWorldJournal, 2014;2014:635240.
PMID: 25250382 DOI: 10.1155/2014/635240

The present research was conducted to discover antimicrobial compounds in methanolic leaf extracts of Jatropha curcas and Andrographis paniculata and ethanolic leaf extract of Psidium guajava and the effectiveness against microbes on flower preservative solution of cut Mokara Red orchid flowers was evaluated. The leaves were analyzed using gas chromatography-mass spectrometry. A total of nine, 66, and 29 compounds were identified in J. curcas, P. guajava, and A. paniculata leaf extracts, with five (88.18%), four (34.66%), and three (50.47%) having unique antimicrobial compounds, respectively. The experimental design on vase life was conducted using a completely randomized design with 10 replications. The flower vase life was about 6 days in the solution containing the P. guajava and A. paniculata leaf extracts at 15 mg/L. Moreover, solution with leaf extracts of A. paniculata had the lowest bacterial count compared to P. guajava and J. curcas. Thus, these leaf extracts revealed the presence of relevant antimicrobial compounds. The leaf extracts have the potential as a cut flower solution to minimize microbial populations and extend flower vase life. However, the activities of specific antimicrobial compounds and double or triple combination leaf extracts to enhance the effectiveness to extend the vase life need to be tested.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods
UPLC method for the determination of vitamin E homologues and derivatives in vegetable oils, margarines and supplement capsules using pentafluorophenyl column

Wong YF, Makahleh A, Saad B, Ibrahim MN, Rahim AA, Brosse N

Talanta, 2014 Dec;130:299-306.
PMID: 25159413 DOI: 10.1016/j.talanta.2014.07.021

A sensitive and rapid reversed-phase ultra performance liquid chromatographic (UPLC) method for the simultaneous determination of tocopherols (α-, β-, γ-, δ-), tocotrienols (α-, β-, γ-, δ-), α-tocopherol acetate and α-tocopherol nicotinate is described. The separation was achieved using a Kinetex pentafluorophenyl (PFP) column (150 × 2.1mm, 2.6 µm) with both photodiode array (PDA) and fluorescence (FL) detectors that were connected in series. Column was thermostated at 42°C. Under a gradient system consisting of methanol and water at a constant flow rate of 0.38 mL min(-1), all the ten analytes were well separated in less than 9.5 min. The method was validated in terms of linearity, limits of detection and quantitation, precision and recoveries. Calibration curves of the ten compounds were well correlated (r(2)>0.999) within the range of 100 to 25,000 μg L(-1) for α-tocopherol acetate and α-tocopherol nicotinate, 10 to 25,000 μg L(-1) for α-tocotrienol and 5 to 25,000 μg L(-1) for the other components. The method is simple and sensitive with detection limits (S/N, 3) of 1.0 to 3.0 μg L(-1) (FL detection) and 30 to 74 μg L(-1) (PDA detection). Relative standard deviations for intra- and inter-day retention times (<1%) and peak areas (≤ 4%) were obtained. The method was successfully applied to the determination of vitamin E in vegetable oils (extra virgin olive, virgin olive, pomace olive, blended virgin and refined olive, sunflower, soybean, palm olein, carotino, crude palm, walnut, rice bran and grape seed), margarines and supplements.

Matched MeSH terms: Chromatography, Liquid; Chromatography, Reverse-Phase

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