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Assessment of 18 endocrine disrupting chemicals in tap water samples from Klang Valley, Malaysia

Haron DEM, Yoneda M, Hod R, Ramli MR, Aziz MY

Environ Sci Pollut Res Int, 2023 Nov;30(51):111062-111075.
PMID: 37801249 DOI: 10.1007/s11356-023-30022-9

Multiclass of endocrine disrupting chemicals (EDCs) such as nine perfluoroalkyl and polyfluoroalkyl substances (PFAS), five bisphenols, and four parabens were analysed in tap water samples from Malaysia's Klang Valley region. All samples were analysed using liquid chromatography mass tandem spectrometry (LC-MS/MS) with limit of quantitation (LOQ) ranged between 0.015 and 5 ng/mL. Fifteen of the 18 EDCs were tested positive in tap water samples, with total EDC concentrations ranging from 0.28 to 5516 ng/L for all 61 sampling point locations. In a specific area of the Klang Valley, the total concentration of EDCs was found to be highest in Hulu Langat, followed by Sepang, Putrajaya, Petaling, Kuala Lumpur, Seremban, and Gombak/Klang. PFAS and paraben were the most found EDCs in all tap water samples. Meanwhile, ethyl paraben (EtP) exhibited the highest detection rate, with 90.2% of all locations showing its presence. Over 60% of the regions showed the presence of perfluoro-n-butanoic acid (PFBA), perfluoro-n-hexanoic acid (PFHXA), perfluoro-n-octanoic acid (PFOA), perfluoro-n-nonanoic acid (PFNA), and perfluoro-1-octanesulfonate (PFOS), whereas the frequency of detection for other compounds was less than 40%. The spatial distribution and mean concentrations of EDCs in the Klang Valley regions revealed that Hulu Langat, Petaling Jaya, and Putrajaya exhibited higher levels of bisphenol A (BPA). On the other hand, Kuala Lumpur and Sepang displayed the highest mean concentrations of PFBA. In the worst scenario, the estimated daily intake (EDI) and risk quotient of some EDCs in this study exceeded the acceptable daily limits recommended by international standards, particularly for BPA, PFOA, PFOS, and PFNA, where the risk quotient (RQ) was found to be greater than 1, indicating a high risk to human health. The increasing presence of EDCs in tap water is undoubtedly a cause for concern as these substances can have adverse health consequences. This highlights the necessity for a standardised approach to evaluating EDC exposure and its direct impact on human populations' health.

Matched MeSH terms: Chromatography, Liquid
Quantification of nimetazepam and its metabolite in human hair samples using liquid chromatography-tandem mass spectrometry: Case report

Dai Y, Han L, Wang Y, Zhao K, Gu J, Bai H, et al.

Leg Med (Tokyo), 2023 Nov;65:102303.
PMID: 37598646 DOI: 10.1016/j.legalmed.2023.102303

Nimetazepam (marketed brand names; Erimin and Lavol) is an intermediate acting benzodiazepine derivative, which was widely used mainly in East and Southeast Asian region countries including Japan, Malaysia, Brunei, the Philippines, Thailand, Indonesia, Hong Kong, Singapore and China. Nimetazepam and its metabolite 7-aminonimetazepam were quantified from human hair samples by liquid chromatography tandem-mass spectrometry (LC-MS/MS), under selective reaction monitoring mode. Using diazepam-d5 as an internal standard, the concentration of nimetazepam and its metabolite 7-aminonimetazepam could be determined by matrix matched calibration method. Extraction of the target compounds was performed by using methanol, followed by evaporation and being concentrated with nitrogen. The Limit of quantification concentrations of nimetazepam and its metabolite 7-aminonimetazepam in hair samples were both 25 pg/mg by established method. The concentrations of nimetazepam in hair samples obtained from 2 users were 27.4, and 22.0 pg/mg, respectively; the concentrations of 7-animonimetazepam in hair samples were 54.2 and 29.1 pg/mg, respectively. In our study, the 7-aminonimetazepam concentrations in hair was higher than those of nimetazepam in the authentic hair samples. To our knowledge, this is the first report to establish the detailed procedure for quantificating nimetazepam and 7-aminonimetazepam in human hair by LC-MS/MS.

Matched MeSH terms: Chromatography, Liquid/methods
Determination of process contaminants 2- and 3-MCPD esters and glycidyl esters in palm-based glycerol by indirect analysis using GC-MS

Ramli NAS, Roslan NA, Abdullah F, Bilal B, Ghazali R, Abd Razak RA, et al.

Food Addit Contam Part A Chem Anal Control Expo Risk Assess, 2023 Oct;40(10):1307-1321.
PMID: 37682685 DOI: 10.1080/19440049.2023.2255290

Esters of 2- and 3-monochloropropanediol (2-MCPDE, 3-MCPDE) and glycidol (GE) are regarded as process contaminants that are found in refined vegetable oils and oil-based foods. Since glycerol is produced during fat splitting, saponification and biodiesel production, it is important to have methods for determining contaminants that might be formed during these processes. Due to the use of glycerol as a food additive, data on the presence of compounds of toxicological concern, including 3-MCPD, are of interest. This study focuses on modifying the indirect analysis of 2-MCPDE, 3-MCPDE and GE using GC-MS based on the AOCS Official Method Cd 29a-13, validating the modified method, and quantifying 2-MCPDE, 3-MCPDE and GE in glycerol. The AOCS Cd 29a-13 method was modified at the initial stage of sample preparation in which the targeted esters were extracted from glycerol by vortex-assisted extraction before sample analysis. This modification was performed based on the polarity of all compounds involved. The calibration functions for all analytes were fitted to linear regression with R2 above 0.99. Limits of detection (LOD) 0.02, 0.01 and 0.02 mg kg-1 were obtained for 2-MCPDE, 3-MCPDE and GE, respectively. Spiked glycerol with 3-MCPDE and 2-MCPDE (0.25, 0.51 and 1.01 mg kg-1) and GE (0.58, 1.16 and 2.32 mg kg-1) were used for recovery and precision measurements. Recoveries of 100-108%, 101-103%, and 93-99% were obtained for 2-MCPDE, 3-MCPDE and GE, respectively. Acceptable precision levels with relative standard deviations ranged from 3.3% to 8.3% were obtained for repeatability and intermediate precision. The validated method was successfully applied for the analysis of the target compounds in refined glycerol from commercial plants, which showed that 2-MCPDE, 3-MCPDE and GE levels in the analysed samples were below the detection limit.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
LC-MS profiling-based non-targeted secondary metabolite screening for deciphering cosmeceutical potential of Malaysian algae

Lim MW, Yow YY, Gew LT

J Cosmet Dermatol, 2023 Oct;22(10):2810-2815.
PMID: 37313630 DOI: 10.1111/jocd.15794

BACKGROUND: Application of natural resources from the marine environment in the cosmeceutical industry is gaining great attention.
AIM: This study pursues to discover the cosmeceutical potential of two Malaysian algae, Sargassum sp. and Kappaphycus sp. by determining their antioxidant capacity and assessing the presence of their secondary metabolites with cosmeceutical potential using non-targeted metabolite profiling.
METHODS: Metabolite profiling using Quadrupole Time-of-Flight (Q-TOF) liquid chromatography-mass spectrometry (LC-MS) in the Electrospray Ionization (ESI) mode resulted in 110 putative metabolites in Sargassum sp. and 47 putative metabolites in Kappaphycus sp. and were grouped according to their functions. To the best of our knowledge, the bioactive compounds of both algae have not been studied in any great detail. This is the first report to explore their cosmeceutical potential.
RESULTS: Six antioxidants were detected in Sargassum sp., including fucoxanthin, (3S, 4R, 3'R)-4-Hydroxyalloxanthin, enzacamene N-stearoyl valine, 2-hydroxy-hexadecanoic acid, and metalloporphyrins. Meanwhile, three antioxidants detected in Kappahycus sp., namely Tanacetol A, 2-fluoro palmitic acid and idebenone metabolites. Three antioxidants are found in both algae species, namely, 3-tert-Butyl-5-methylcatechol, (-)-isoamijiol, and (6S)-dehydrovomifoliol. Anti-inflammatory metabolites such as 5(R)-HETE, protoverine, phytosphingosine, 4,5-Leukotriene-A4, and 5Z-octadecenoic acid were also found in both species. Sargassum sp. possesses higher antioxidant capacity as compared to Kappahycus sp. which may be linked to its number of antioxidant compounds found through LC-MS.
CONCLUSIONS: Hence, our results conclude that Malaysian Sargassum sp. and Kappaphycus sp. are potential natural cosmeceutical ingredients as we aim to produce algae cosmeceutical products using native algae.

Matched MeSH terms: Chromatography, Liquid/methods
Fulltext Ethanolic Extract of Polygonum minus Protects Differentiated Human Neuroblastoma Cells (SH-SY5Y) against H2O2-Induced Oxidative Stress

Sayuti NH, Zulkefli N, Tan JK, Saad N, Baharum SN, Hamezah HS, et al.

Molecules, 2023 Sep 20;28(18).
PMID: 37764502 DOI: 10.3390/molecules28186726

Neuronal models are an important tool in neuroscientific research. Hydrogen peroxide (H2O2), a major risk factor of neuronal oxidative stress, initiates a cascade of neuronal cell death. Polygonum minus Huds, known as 'kesum', is widely used in traditional medicine. P. minus has been reported to exhibit a few medicinal and pharmacological properties. The current study aimed to investigate the neuroprotective effects of P. minus ethanolic extract (PMEE) on H2O2-induced neurotoxicity in SH-SY5Y cells. LC-MS/MS revealed the presence of 28 metabolites in PMEE. Our study showed that the PMEE provided neuroprotection against H2O2-induced oxidative stress by activating the Nrf2/ARE, NF-κB/IκB and MAPK signaling pathways in PMEE pre-treated differentiated SH-SY5Y cells. Meanwhile, the acetylcholine (ACH) level was increased in the oxidative stress-induced treatment group after 4 h of exposure with H2O2. Molecular docking results with acetylcholinesterase (AChE) depicted that quercitrin showed the highest docking score at -9.5 kcal/mol followed by aloe-emodin, afzelin, and citreorosein at -9.4, -9.3 and -9.0 kcal/mol, respectively, compared to the other PMEE's identified compounds, which show lower docking scores. The results indicate that PMEE has neuroprotective effects on SH-SY5Y neuroblastoma cells in vitro. In conclusion, PMEE may aid in reducing oxidative stress as a preventative therapy for neurodegenerative diseases.

Matched MeSH terms: Chromatography, 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
The anti-allergic potential of stingless bee honey from different botanical sources via modulation of mast cell degranulation

Yong PYA, Yip AJW, Islam F, Hong HJ, Teh YE, Tham CL, et al.

BMC Complement Med Ther, 2023 Sep 04;23(1):307.
PMID: 37667314 DOI: 10.1186/s12906-023-04129-y

BACKGROUND: Allergy is an inflammatory disorder affecting around 20% of the global population. The adverse effects of current conventional treatments give rise to the increased popularity of using natural food products as complementary and alternative medicine against allergic diseases. Stingless bee honey, commonly known as Kelulut honey (KH) in Malaysia, has been used locally as a traditional remedy to relieve cough and asthma. This study evaluated the anti-allergic potential of KH collected from four different botanical sources on phorbol ester 12-myristate-3-acetate and calcium ionophore-activated human mast cells.
METHODS: The present study examined the inhibitory effects of all collected honey on the release of selected inflammatory mediators, such as tumor necrosis factor-α (TNF-α), interleukin (IL)-4, IL-6, IL-8, histamine, and β-hexosaminidase in an activated HMC. Besides that, all honey's total phenolic content (TPC) was also examined, followed by using liquid chromatography with tandem mass spectrometry (LC-MS/MS) to identify the phytochemicals in the honey. Further examination of the identified phytochemicals on their potential interaction with selected signaling molecules in an activated mast cell was conducted using computational methods.
RESULTS: The results indicated that there were significant inhibitory effects on all selected inflammatory mediators' release by KH sourced from bamboo (BH) and rubber tree (RH) at 0.5% and 1%, but not KH sourced from mango (AH) and noni (EH). BH and RH were found to have higher TPC values and were rich in their phytochemical profiles based on the LC-MS/MS results. Computational studies were employed to determine the possible molecular target of KH through molecular docking using HADDOCK and PRODIGY web servers.
CONCLUSIONS: In short, the results indicated that KH possesses anti-allergic effects towards an activated HMC, possibly by targeting downstream MAPKs. However, their anti-allergic effects may vary according to their botanical sources. Nevertheless, the present study has provided insight into the potential application of stingless bee honey as a complementary and alternative medicine to treat various allergic diseases.

Matched MeSH terms: Chromatography, Liquid
Fulltext Quantitative proteomics analysis of permethrin and temephos-resistant Ae. aegypti revealed diverse differentially expressed proteins associated with insecticide resistance from Penang Island, Malaysia

Shettima A, Ishak IH, Lau B, Abu Hasan H, Miswan N, Othman N

PLoS Negl Trop Dis, 2023 Sep;17(9):e0011604.
PMID: 37721966 DOI: 10.1371/journal.pntd.0011604

Synthetic insecticides are the primary vector control method used globally. However, the widespread use of insecticides is a major cause of insecticide-resistance in mosquitoes. Hence, this study aimed at elucidating permethrin and temephos-resistant protein expression profiles in Ae. aegypti using quantitative proteomics. In this study, we evaluated the susceptibility of Ae. aegypti from Penang Island dengue hotspot and non-hotspot against 0.75% permethrin and 31.25 mg/l temephos using WHO bioassay method. Protein extracts from the mosquitoes were then analysed using LC-ESI-MS/MS for protein identification and quantification via label-free quantitative proteomics (LFQ). Next, Perseus 1.6.14.0 statistical software was used to perform differential protein expression analysis using ANOVA and Student's t-test. The t-test selected proteins with≥2.0-fold change (FC) and ≥2 unique peptides for gene expression validation via qPCR. Finally, STRING software was used for functional ontology enrichment and protein-protein interactions (PPI). The WHO bioassay showed resistance with 28% and 53% mortalities in adult mosquitoes exposed to permethrin from the hotspot and non-hotspot areas. Meanwhile, the susceptibility of Ae. aegypti larvae revealed high resistance to temephos in hotspot and non-hotspot regions with 80% and 91% mortalities. The LFQ analyses revealed 501 and 557 (q-value <0.05) differentially expressed proteins in adults and larvae Ae. aegypti. The t-test showed 114 upregulated and 74 downregulated proteins in adult resistant versus laboratory strains exposed to permethrin. Meanwhile, 13 upregulated and 105 downregulated proteins were observed in larvae resistant versus laboratory strains exposed to temephos. The t-test revealed the upregulation of sodium/potassium-dependent ATPase β2 in adult permethrin resistant strain, H15 domain-containing protein, 60S ribosomal protein, and PB protein in larvae temephos resistant strain. The downregulation of troponin I, enolase phosphatase E1, glucosidase 2β was observed in adult permethrin resistant strain and tubulin β chain in larvae temephos resistant strain. Furthermore, the gene expression by qPCR revealed similar gene expression patterns in the above eight differentially expressed proteins. The PPI of differentially expressed proteins showed a p-value at <1.0 x 10-16 in permethrin and temephos resistant Ae. aegypti. Significantly enriched pathways in differentially expressed proteins revealed metabolic pathways, oxidative phosphorylation, carbon metabolism, biosynthesis of amino acids, glycolysis, and citrate cycle. In conclusion, this study has shown differentially expressed proteins and highlighted upregulated and downregulated proteins associated with insecticide resistance in Ae. aegypti. The validated differentially expressed proteins merit further investigation as a potential protein marker to monitor and predict insecticide resistance in field Ae. aegypti. The LC-MS/MS data were submitted into the MASSIVE database with identifier no: MSV000089259.

Matched MeSH terms: Chromatography, Liquid
Antidepressant evaluation of Andrographis paniculata Nees extract and andrographolide in chronic unpredictable stress zebrafish model

Aldurrah Z, Mohd Kauli FS, Abdul Rahim N, Zainal Z, Afzan A, Al Zarzour RH, et al.

Comp Biochem Physiol C Toxicol Pharmacol, 2023 Sep;271:109678.
PMID: 37301417 DOI: 10.1016/j.cbpc.2023.109678

Andrographis paniculata (A. paniculata) showed an anti-depressive effect in rodent models. Zebrafish has recently emerged as a worthy complementary translational model for antidepressant drug discovery study. This study investigates the anti-depressive effect of A. paniculata extract and andrographolide in the chronic unpredictable stress (CUS)- zebrafish model. Four groups of zebrafish (n = 10/group), i.e. control, CUS (stressed, untreated), CUS + A. paniculata (100 mg/L) and CUS + fluoxetine (0.01 mg/L) were assessed in open-field and social interaction tests, 24 h after treatment. After extract screening, behavioural and cortisol analysis of andrographolide (5, 25 and 50 mg/kg, i.p.) and fluoxetine (10 mg/kg, i.p.) were evaluated. Before the behavioural study, acute toxicity and characterization of A. paniculata extract using UHPLC-ESI-MS/MS were performed. A significant reduction in freezing duration was found in A. paniculata- (t-test, p = 0.0234) and fluoxetine-treated groups (t-test, p

Matched MeSH terms: Chromatography, Liquid
A review on the occurrence, analytical methods, and impact of microplastics in the environment

Tran TV, Jalil AA, Nguyen TM, Nguyen TTT, Nabgan W, Nguyen DTC

Environ Toxicol Pharmacol, 2023 Sep;102:104248.
PMID: 37598982 DOI: 10.1016/j.etap.2023.104248

Nowadays, microplastic pollution is one of the globally urgent concerns as a result of discharging plastic products into the atmosphere, aquatic and soil environments. Microplastics have average size of less than 5 mm, are non-biodegradable, accumulative, and highly persistent substances. Thousands of tons of microplastics are still accumulated in various environments, posing an enormous threat to human health and living creatures. Here, we review the occurrence and analytical methods, and impact of microplastics in the environments including soil, aquatic media, and atmosphere. Analytical methods including visual observation, Fourier-transform infrared spectroscopy, Raman spectroscopy, scanning electron microscopy, and pyrolysis-gas chromatography-mass spectrometry were evaluated. We elucidated the environmental and human health impacts of microplastics with emphasis on life malfunction, immune disruption, neurotoxicity, diseases and other tangible health risks. This review also found some shortages of analytical equivalence and/or standardization, inconsistence in sampling collection and limited knowledge of microplastic toxicity. It is hopeful that the present work not only affords a more insight into the potential dangers of microplastics on human health but also urges future researches to establish new standardizations in analytical methods.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
A simple and high efficiency purification of His-tagged turnip yellow mosaic virus-like particle (TYMV-VLP) by nickel ion affinity precipitation

Tan FH, Ng JF, Mohamed Alitheen NB, Muhamad A, Yong CY, Lee KW

J Virol Methods, 2023 Sep;319:114771.
PMID: 37437780 DOI: 10.1016/j.jviromet.2023.114771

Virus-like particles (VLPs) is one of the most favourable subjects of study, especially in the field of nanobiotechnology and vaccine development because they possess good immunogenicity and self-adjuvant properties. Conventionally, VLPs can be tagged and purified using affinity chromatography or density gradient ultracentrifugation which is costly and time-consuming. Turnip yellow mosaic virus (TYMV) is a plant virus, where expression of the viral coat protein (TYMVc) in Escherichia coli (E. coli) has been shown to form VLP. In this study, we report a non-chromatographic method for VLP purification using C-terminally His-tagged TYMVc (TYMVcHis6) as a protein model. Firstly, the TYMVcHis6 was cloned and expressed in E. coli. Upon clarification of cell lysate, nickel (II) chloride [NiCl2; 15 µM or equivalent to 0.0000194% (w/v)] was added to precipitate TYMVcHis6. Following centrifugation, the pellet was resuspended in buffer containing 1 mM EDTA to chelate Ni2+, which is then removed via dialysis. A total of 50% of TYMVcHis6 was successfully recovered with purity above 0.90. Later, the purified TYMVcHis6 was analysed with sucrose density ultracentrifugation, dynamic light scattering (DLS), and transmission electron microscopy (TEM) to confirm VLP formation, which is comparable to TYMVcHis6 purified using the standard immobilized metal affinity chromatography (IMAC) column. As the current method omitted the need for IMAC column and beads while significantly reducing the time needed for column washing, nickel affinity precipitation represents a novel method for the purification of VLPs displaying poly-histidine tags (His-tags).

Matched MeSH terms: Chromatography, Affinity/methods
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
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 Protein Profiling of Aedes aegypti Treated with Streptomyces sp. KSF103 Ethyl Acetate Extract Reveals Potential Insecticidal Targets and Metabolic Pathways

Tan KS, Azman AS, Hassandarvish P, Amelia-Yap ZH, Tan TK, Low VL

Int J Mol Sci, 2023 Aug 03;24(15).
PMID: 37569772 DOI: 10.3390/ijms241512398

The insecticidal activity of Streptomyces sp. KSF103 ethyl acetate (EA) extract against mosquitoes is known; however, the underlying mechanism behind this activity remains elusive. In this study, liquid chromatography with tandem mass spectrometry (LC-MS/MS) was employed to investigate changes in the protein profile of Aedes aegypti larvae and adults treated with lethal concentrations of 50 (LC50) EA extract. By comparing the treated and untreated mosquitoes, this study aimed to identify proteins or pathways that exhibit alterations, potentially serving as targets for future insecticide development. Treatment with a lethal concentration of EA extract upregulated 15 proteins in larvae, while in adults, 16 proteins were upregulated, and two proteins were downregulated. These proteins were associated with metabolism, protein regulation/degradation, energy production, cellular organization and structure, enzyme activity, and catalysis, as well as calcium ion transport and homeostasis. Notably, ATP synthase, fructose-bisphosphate aldolase (FBA), and ATP citrate synthase were significantly expressed in both groups. Gene ontology analysis indicated a focus on energy metabolic processes. Molecular docking revealed a strong interaction between dodemorph, selagine (compounds from the EA extract), and FBA, suggesting FBA as a potential protein target for insecticide development. Further studies such as Western blot and transcriptomic analyses are warranted to validate the findings.

Matched MeSH terms: Chromatography, Liquid
Size-exclusion chromatography for the characterization of urinary extracellular vesicles

Park S, Jalaludin I, Hwang H, Ko M, Adelipour M, Hwan M, et al.

J Chromatogr B Analyt Technol Biomed Life Sci, 2023 Aug 01;1228:123828.
PMID: 37480686 DOI: 10.1016/j.jchromb.2023.123828

In recent years, extracellular vesicles (EVs) have gained attention for their potential as biomarkers for the early diagnosis and treatment of various diseases. Traditionally, EV isolation has relied exclusively on ultracentrifugation. However, alternative enrichment methods such as size-exclusion chromatography (SEC) and polyethylene glycol-based precipitation have been introduced. This study utilized SEC as a characterization tool to assess the efficiency of EV isolation. Urinary EVs isolated from human urine using centrifugation (40,000 × g) were analyzed using an SEC column with a pore size of 1000 Å, an inner diameter of 7.8 mm, and a length of 300 mm. The EVs were detected sequentially using UV (280 nm) and fluorescence (λex/em = 550 nm/565 nm); the EVs were observed at approximately 6 min, while the proteins were observed at approximately 12 min. The repeated centrifugation enrichment steps resulted in an increase in EV peaks and a decrease in protein peaks. SEC analysis of the enriched EV samples confirmed that a four-cycle repetition of centrifugation is necessary for successful EV enrichment and removal of non-EV proteins from 40 mL of human urine.

Matched MeSH terms: Chromatography, Gel
Essential oil composition, anti-tyrosinase activity, and molecular docking studies of Knema intermedia Warb. (Myristicaceae)

Salihu AS, Salleh WMNHW, Setzer WN

Z Naturforsch C J Biosci, 2023 Jul 26;78(7-8):293-298.
PMID: 36960928 DOI: 10.1515/znc-2023-0003

Knema is one of the genera in the Myristicaceae family. The genus includes 60 species in Southeast Asia and is traditionally used for treating skin disorders. Here, for the first time, the essential oil, anti-tyrosinase, and molecular docking studies of Knema intermedia were evaluated. The essential oil was obtained by hydrodistillation and fully characterized by gas chromatography (GC-FID) and gas chromatography-mass spectrometry (GC-MS). Anti-tyrosinase activity was evaluated against mushroom tyrosinase, whereas molecular docking studies were performed using Autodock vina embedded in PyRx to evaluate the binding interactions of major components. A total of 37 components (97.3%) were successfully identified in the essential oil, which was characterized by high amounts of t-muurolol (20.1%), α-copaene (14.4%), δ-cadinene (13.9%), germacrene B (9.5%), and δ-selinene (7.0%). The essential oil displayed moderate inhibitory activity towards tyrosinase with an IC50 value of 70.2 μg/mL. The best docking energy was observed with δ-selinene (-7.8 kcal/mol), and it also forms interactions with His85, His263, and His244 which are important amino acid residues of the tyrosinase receptor. Hence, this study provides valuable scientific data on K. intermedia as potential candidate for the development of natural antiaging formulations.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fulltext The Effects of 12 Weeks Colostrum Milk Supplementation on the Expression Levels of Pro-Inflammatory Mediators and Metabolic Changes among Older Adults: Findings from the Biomarkers and Untargeted Metabolomic Analysis

Ooi TC, Ahmad A, Rajab NF, Sharif R

Nutrients, 2023 Jul 18;15(14).
PMID: 37513601 DOI: 10.3390/nu15143184

Senescence is a normal biological process that is accompanied with a series of deteriorations in physiological function. This study aimed to investigate the effects of bovine colostrum milk supplementation on metabolic changes and the expression of various biomarkers on inflammation, antioxidant and oxidative damage, nutrient metabolism, and genomic stability among older adults. Older adults (50-69 years old) who participated in the 12-week randomized, double-blinded, placebo-controlled trial were instructed to consume the IgCo bovine colostrum-enriched skim milk or regular skim milk (placebo) twice daily. Following 12 weeks of intervention, participants in the intervention group had lower expression levels in pro-inflammatory mediators (CRP, IL-6, and TNF-α), with significant (p < 0.05) interaction effects of the group and time observed. However, no significant interaction effect was observed in the vitamin D, telomerase, 8-OHdG, MDA, and SOD activities. UPLC-MS-based untargeted metabolomics analysis revealed that 22 metabolites were upregulated and 11 were downregulated in the intervention group compared to the placebo group. Glycerophospholipid metabolism, along with cysteine and methionine metabolism were identified as the potential metabolic pathways that are associated with bovine colostrum milk consumption. In conclusion, consuming bovine colostrum milk may induce metabolic changes and reduce the expression of various pro-inflammatory mediators, thus improving the immune function in older adults.

Matched MeSH terms: Chromatography, Liquid
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
An integrative GC-MS and LC-MS metabolomics platform determination of the metabolite profile of Bombax ceiba L. root, and in silico & in vitro evaluation of its antibacterial & antidiabetic activities

Alrabie A, Alrabie NA, AlSaeedy M, Al-Adhreai A, Al-Qadsy I, Al-Horaibi SA, et al.

Nat Prod Res, 2023 Jul;37(13):2263-2268.
PMID: 36441059 DOI: 10.1080/14786419.2022.2149519

The Bombax ceiba L. tree is a member of the family Bombacaceae and the genus Bombax. Both Chinese and Indian traditional medicine have made extensive use of it in the treatment of sickness. Its chemical composition is still a mystery. B. ceiba roots methanol extract (BCRME) was analyzed by different chromatographic analytical techniques in order to identify its major chemical constituents. Twelve compounds and six compounds were identified from GC-MS and LC-MS analysis, respectively. This is the first report on the presence of lathodoratin, cedrene, 4H-1-benzopyran-4-one,8-[{dimethylamino} methyl]-7-methoxy-3-methyl-2-phenyl, asiatic acid, and (E)-2,4,4'-trihydroxylchalcone in B. ceiba roots. Methanol extract demonstrated noteworthy antibacterial activity against Staphylococcus aureus (MTCC96) (MIC: 100 µg/mL) compare to antibiotic ampicillin (MIC: 250 µg/mL) as well as the highest α-amylase inhibition (IC50=26.91 µg/mL) and α-glucosidase inhibition (IC50=21.21 µg/mL) effects, molecular docking study confirmed these findings, with some compounds having a very high docking score.

Matched MeSH terms: Chromatography, Liquid; Gas Chromatography-Mass Spectrometry
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

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