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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.
Fulltext Pain relief with intravenous regional guanethedine in post-traumatic reflex sympathetic dystrophy--a case report

Vijayan R, Low KH

Med J Malaysia, 1993 Jun;48(2):236-9.
PMID: 8350804

Intravenous regional guanethedine (IVRG), using the Bier's block technique, was given to relieve pain in a 62 year old Indian woman suffering from reflex sympathetic dystrophy. The patient obtained complete pain relief with 2 injections and has remained pain-free for 18 months.
Effect of PEGylated lipid and Lecinol S-10 on physico-chemical properties and encapsulation efficiency of palmitoleate-palmitoleic acid vesicles

Teo YY, Misran M, Low KH

J Liposome Res, 2014 Sep;24(3):241-8.
PMID: 24597523 DOI: 10.3109/08982104.2014.891234

A vesicle is a microscopic particle composed of a lipid bilayer membrane that separates the inner aqueous compartment from the outer aqueous environment. Palmitoleate-palmitoleic acid vesicles were prepared and their physico-chemical properties were investigated. Moreover, mixed vesicles composed of palmitoleic acid and PEGylated lipid and/or a mixture of phospholipids were also prepared. The stabilizing effects of these double-chain lipids on the formation of palmitoleate-palmitoleic acid vesicles were studied. Stability of the vesicle suspension was examined using particle size and zeta potential at 30 °C. The magnitude of the zeta potential was relatively lower in the vesicle suspension with the presence of phospholipid. Although some of the mixed vesicles that were formed were not very stable, they displayed potential for encapsulating the active ingredient calcein and the encapsulation efficiencies of calcein were encouraging. The palmitoleate-palmitoleic acid-DPPE-PEG2000 vesicle showed the most promising stability and encapsulation efficiency.
Differential-based biosensor array for fluorescence-chemometric discrimination and the quantification of subtle chloropropanols by cross-reactive serum albumin scaffolding

Wong SF, Low KH, Khor SM

Talanta, 2020 Oct 01;218:121169.
PMID: 32797922 DOI: 10.1016/j.talanta.2020.121169

Food contamination is a serious concern because of a high level of chemicals in food causes severe health issues. Safeguarding the public from the risk of adulterated foods has become a challenging mission. Chloropropanols are of importance to food safety and food security because they are common chemical food contaminants and believed to be carcinogenic to humans. In chemical sensing, chloropropanols are challenging analytes owing to the lacking diversity of functional groups and difficulty in targeting the hydroxyl group in aqueous environments. Moreover, because of their small molecular size, the compositions of chloropropanols remain challenging for achieving chromatographic determination. Herein, to simulate human smell and taste sensations, serum albumins, which are protein-based receptors, were introduced as low-selective receptors for differential sensing. Utilizing serum albumins, a fluorophore (PRODAN), and an additive (ascorbic acid), a differential-based optical biosensor array was developed to detect and differentiate chloropropanols. By integrating the sensor array with linear discriminant analysis (LDA), four chloropropanols were effectively differentiated based on their isomerism properties and the number of the hydroxyl groups, even at ultra-low concentration (5 nM). This concentration is far below the maximum tolerable level of 0.18 μM for chloropropanols. The sensing array was then employed for chloropropanols differentiation and quantification in the complex mixtures (e.g., synthetic soy and dark soy sauces). Leave-one-out cross-validation (LOOCV) analysis demonstrated 100% accurate classification for all tests. These results signify our differential sensing array as a practical and powerful tool to speedily identify, differentiate, and even quantify chloropropanols in food matrices.
Exploring the potential of Fe(III)-EGTA and Fe(III)-DTPA as the catalysts to enhance UV/persulfate in the degradation of aqueous sulfamethazine

Ng KA, Low KH, Tay KS

Water Environ Res, 2023 Apr;95(4):e10862.
PMID: 37032435 DOI: 10.1002/wer.10862

The combination of UV and water-soluble Fe(III) complexes is an effective method for generating Fe(II) in situ for activating advanced oxidation processes. This study explored the potential of Fe(III)-diethylenetriaminepentaacetic acid (Fe(III)-DTPA) and Fe(III)-ethylene glycol-bis(2-aminoethylether)-N,N,N',N'-tetraacetic acid (Fe(III)-EGTA) in activating the UV/persulfate (UV/PS) for sulfamethazine removal. The initial screening showed that Fe(III)-EGTA and Fe(III)-DTPA could significantly improve the rate of sulfamethazine removal. The optimum molar ratios of persulfate to Fe(III)-DTPA and Fe(III)-EGTA were 100:1 and 100:2.5. The predicted percentage of sulfamethazine removal under the optimized conditions, obtained using response surface methodology, was ~99% for both catalysts. The pH range of 6 to 8 did not significantly affect the performance of UV/PS in the removal of sulfamethazine. The percentage sulfamethazine removal in the selected water samples was ranged from 93.6% to 99.6%, agreeing with the predicted value. The performance of both catalysts in activating UV/PS is comparable with that of the frequently used Fe(III)-EDDS. PRACTITIONERS POINTS: The potential of Fe(III)-DTPA and Fe(III)-EGTA in activating UV/persulfate (UV/PS) was explored. Fe(III)-DTPA and Fe(III)-EGTA improved the performance of UV/PS in sulfamethazine removal. Fe(III)-DTPA and Fe(III)-EGTA are effective in catalyzing UV/PS under pH 6 to 8. The performance of Fe(III)-DTPA and Fe(III)-EGTA is comparable with well-studied Fe(III)-EDDS.
Distribution and health risk assessment of trace metals in freshwater tilapia from three different aquaculture sites in Jelebu Region (Malaysia)

Low KH, Zain SM, Abas MR, Md Salleh K, Teo YY

Food Chem, 2015 Jun 15;177:390-6.
PMID: 25660902 DOI: 10.1016/j.foodchem.2015.01.059

The trace metal concentrations in edible muscle of red tilapia (Oreochromis spp.) sampled from a former tin mining pool, concrete tank and earthen pond in Jelebu were analysed with microwave assisted digestion-inductively coupled plasma-mass spectrometry. Results were compared with established legal limits and the daily ingestion exposures simulated using the Monte Carlo algorithm for potential health risks. Among the metals investigated, arsenic was found to be the key contaminant, which may have arisen from the use of formulated feeding pellets. Although the risks of toxicity associated with consumption of red tilapia from the sites investigated were found to be within the tolerable range, the preliminary probabilistic estimation of As cancer risk shows that the 95th percentile risk level surpassed the benchmark level of 10(-5). In general, the probabilistic health risks associated with ingestion of red tilapia can be ranked as follows: former tin mining pool > concrete tank > earthen pond.
Comparison of unmodified and modified BCR sequential extraction schemes for the fractionation of heavy metals in shrimp aquaculture sludge from Selangor, Malaysia

Nemati K, Abu Bakar NK, Abas MR, Sobhanzadeh E, Low KH

Environ Monit Assess, 2011 May;176(1-4):313-20.
PMID: 20632089 DOI: 10.1007/s10661-010-1584-3

A study was carried out to investigate the fractionation of Cd, Cr, Cu, Fe, Mn, Pb, and Zn in shrimp aquaculture sludge from Selangor, Malaysia, using original (unmodified) and modified four-steps BCR (European Community Bureau of Reference, now known as the Standards Measurements and Testing Program) sequential extraction scheme. Step 2 of the unmodified BCR procedure (subsequently called Method A) involves treatment with 0.1 M hydroxylammonium chloride at pH 2, whereas 0.5 M hydroxylammonium chloride at pH 1.5 was used in the modified BCR procedure (subsequently called Method B). Metal analyses were carried out by flame atomic absorption spectrometry. A pseudo-total aqua-regia digest of BCR CRM 701 has also been undertaken for quality assurance purposes. The recovery of Method A for all metals studied ranges from 96.14% to 105.26%, while the recovery for Method B ranges from 95.94% to 122.40%. Our results reveal that Method A underestimated the proportion of metals bound to the easily reducible fraction except for copper. Therefore, the potential mobility of these elements is higher than others. Thus, to use this sludge as a fertilizer we have to first find a remediation for reduction of heavy metal contamination.
Comparative study on open system digestion and microwave assisted digestion methods for metal determination in shrimp sludge compost

Nemati K, Abu Bakar NK, Bin Abas MR, Sobhanzadeh E, Low KH

J Hazard Mater, 2010 Oct 15;182(1-3):453-9.
PMID: 20638781 DOI: 10.1016/j.jhazmat.2010.06.053

The aim of this work was to evaluate two different digestion methods for the determination of the total concentration of metals (Zn, Cu, Cr, Ni, Pb and Cd) in shrimp sludge compost. The compost made from shrimp aquaculture sludge co-composted with organic materials (peat, crushed bark and manure) was used as an organic growing medium for crop. Open system digestion and microwave assisted digestion procedures were employed in sample preparation. Various combinations and volumes of hydrofluoric, nitric and hydrochloric acids were evaluated for the efficiency of both methods. A certified reference material (CRM 146) was used in the comparison of these two digestion methods. The results revealed a good agreement between both procedures and the certified valued. The best recoveries were found in the range between 95% and 99% for microwave assisted digestion with a mixture of 2 ml of HF, 6 ml of HNO(3) and 2 ml of HCl. This procedure was recommended as the method for digestion the compost herein based on the recovery analysis and time taken.
H emibagrus sp. as a potential bioindicator of hazardous metal pollution in Selangor River

Idris NSU, Low KH, Koki IB, Kamaruddin AF, Md Salleh K, Zain SM

Environ Monit Assess, 2017 May;189(5):220.
PMID: 28425070 DOI: 10.1007/s10661-017-5939-x

The spatial distributions of Na, Mg, K, Ca, Cr, Fe, Ni, Cu, Zn, As, Se and Pb in Hemibagrus sp. from Selangor River and a reference site were determined with inductively coupled plasma-mass spectrometer, in comparison to the levels in their surrounding water body and sediments. The results demonstrated significant differences in elemental accumulation pattern in different fish tissues originated from both sites. The variations observed were mainly subjected to their metabolic activities, and also the influence of the surrounding medium. In general, the liver tends to accumulate higher concentration of metals followed by the gills, and muscle tissues. The data also indicate associations between the concentrations of metal contaminants measured in the fish and the levels observed at the sites. The concentrations of hazardous metals As, Se and Pb in all the studied tissues reflect the influence of anthropogenic inputs. This suggests the potential utility of widely available Hemibagrus sp. as a valuable bioindicator of metal pollution in environmental monitoring and assessment.
Estimation of the dietary intake and risk assessment of food carcinogens (3-MCPD and 1,3-DCP) in soy sauces by Monte Carlo simulation

Wong SF, Lee BQ, Low KH, Jenatabadi HS, Wan Mohamed Radzi CWJB, Khor SM

Food Chem, 2020 May 01;311:126033.
PMID: 31869642 DOI: 10.1016/j.foodchem.2019.126033

Quantifiable levels of 3-chloropropane-1,2-diol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) were found in domestically manufactured soy-based sauces. Selected commercial foods in the Malaysian market (n = 43) were analyzed for their 3-MCPD and 1,3-DCP contents using a validated gas chromatography-mass spectrometry technique. The 3-MCPD and 1,3-DCP contents of the analyzed food samples varied from not detectable levels to 0.1223 ± 0.0419 mg kg-1 and not detectable levels to 0.025 ± 0.0041 mg kg-1, respectively. High concentrations of 3-MCPD, exceeding Malaysia's maximum tolerable limit of 0.02 mg kg-1, were found in chicken seasoning cubes (mean = 0.0898 ± 0.0378 mg kg-1). Monte Carlo simulation-based health risk assessment revealed that 3-MCPD and 1,3-DCP intakes in the 50th, 95th, and 99th percentiles were lower than 4 µg kg-1 bw day-1, the limit recommended by JECFA in 2016. Hence, it was concluded that the exposure of Malaysian citizens to chloropropanols through soy sauce consumption does not present a health risk.
Assessment of denitrification potential for coastal and inland sites using groundwater and soil analysis: the multivariate approach

Dahiru M, Abu Bakar NK, Yus Off I, Low KH, Mohd MN

Environ Monit Assess, 2020 Apr 19;192(5):294.
PMID: 32307605 DOI: 10.1007/s10661-020-08276-4

In an effort to determine the reason behind excellent nitrate remediation capacity at Kelantan region, a multivariate approach is employed to evaluate extent to which the influence of sea on soil geochemical composition affect variation pattern of groundwater quality. The results obtained from geochemical analysis of paleo-beach soil in coastal site at Bachok revealed multiple redox activity at different soil strata, involving both heterotrophic and autotrophic denitrification. In soil and water analysis, eight of the fourteen hydro-geochemical parameters (conductivity, temperature, soil texture, oxidation reduction potential, pH, total organic carbon, Fe, Cu, Mn, Cl-, SO42-, NO2-, NO3- and PO43-) measured using standard procedures were subjected to multivariate analysis. Evaluation of general variation pattern across the area reveals that the principal component analysis (PCA), hierarchical cluster analysis (HCA) and linear discriminant analysis (LDA) are in consonance with one another on apportioning three parameters (SO42-, Cl- and conductivity) to the coastal sites and two parameters (Fe and NH4+ or NO3-) to inland sites. The step forward analysis of LDA reveals four parameters in order of decreasing significance as Cl-, Fe and SO42-, while the two-way HCA identifies three clusters on location basis, respectively. In addition to the significant data reduction obtained, the results indicate that proximity to sea and location/geological-based influence are more significant than temporal-based influence in denitrification. By extension, the research reveals that influence of labile portion of natural resources is explorable for broader application in other remediation strategies.
Consumption of water from ex-mining ponds in Klang Valley and Melaka, Malaysia: A health risk study

Koki IB, Low KH, Juahir H, Abdul Zali M, Azid A, Zain SM

Chemosphere, 2018 Mar;195:641-652.
PMID: 29287272 DOI: 10.1016/j.chemosphere.2017.12.112

Evaluation of health risks due to heavy metals exposure via drinking water from ex-mining ponds in Klang Valley and Melaka has been conducted. Measurements of As, Cd, Pb, Mn, Fe, Na, Mg, Ca, and dissolved oxygen, pH, electrical conductivity, total dissolved solid, ammoniacal nitrogen, total suspended solid, biological oxygen demand were collected from 12 ex-mining ponds and 9 non-ex-mining lakes. Exploratory analysis identified As, Cd, and Pb as the most representative water quality parameters in the studied areas. The metal exposures were simulated using Monte Carlo methods and the associated health risks were estimated at 95th and 99th percentile. The results revealed that As was the major risk factor which might have originated from the previous mining activity. For Klang Valley, adults that ingested water from those ponds are at both non-carcinogenic and carcinogenic risks, while children are vulnerable to non-carcinogenic risk; for Melaka, only children are vulnerable to As complications. However, dermal exposure showed no potential health consequences on both adult and children groups.
Correlation of chemical profiles obtained from 1 H-NMR and LC-MS metabolomics with α-glucosidase inhibition activity for varietal selections of Ficus deltoidea

Kasim N, Afzan A, Mediani A, Low KH, Ali AM, Mat N, et al.

Phytochem Anal, 2022 Dec;33(8):1235-1245.
PMID: 36192845 DOI: 10.1002/pca.3175

INTRODUCTION: Ficus deltoidea Jack (Moraceae) is a plant used in Malaysia to treat various ailments, including diabetes. The presence of several varieties raises essential questions regarding which is the potential bioactive variety and what are the bioactive metabolites.
OBJECTIVES: Here, we explored the phytochemical diversity of the seven varieties from Peninsular Malaysia using Nuclear Magnetic Resonance (NMR) and Liquid Chromatography-Mass Spectrometry (LC-MS) analyses and correlated it with the α-glucosidase inhibitory activity.
METHODOLOGY: The Nuclear Overhauser Effect Spectroscopy (NOESY) One-Dimensional (1D)-NMR and LC-MS data were processed, annotated, and correlated with in vitro α-glucosidase inhibitory using multivariate data analysis.
RESULTS: The α-glucosidase results demonstrated that different varieties have varying inhibitory effects, with the highest inhibition rate being F. deltoidea var. trengganuensis and var. kunstleri. Furthermore, diverse habitats and plant ages could also influence the inhibitory rate. The heat map from NMR and LC-MS profiles showed unique patterns according to varying levels of α-glucosidase inhibition rate. The Partial Least Squares (PLS) model constructed from both NMR and LC-MS further confirmed the correlation between the α-glucosidase inhibition rate of F. deltoidea varieties and its metabolite profiles. The Variable Influence on Projection (VIP) and correlation coefficient (p(corr)) values values were used to determine the highly relevant metabolites for explaining the anticipated inhibitory action.
CONCLUSION: NMR and LC-MS annotations allow the identification of flavan-3-ols and proanthocyanidins as the key bioactive factors. Our current results demonstrated the value of multivariate data analysis to predict the quality of herbal materials from both biological and chemical aspects.
Rapid and nondestructive analysis of lipstick on different substrates using ATR-FTIR spectroscopy and chemometrics

Ka Khei L, Verma R, Tan ELY, Low KH, Ismail D, Mohamad Asri MN

J Forensic Sci, 2023 Feb 15.
PMID: 36789805 DOI: 10.1111/1556-4029.15223

Lipstick can be an important piece of evidence in crimes like murders, rapes, and suicides. Due to its prevalence, it can be an important corroborative evidence in crime reconstruction. The analysis of such evidence can provide an evidentiary link between the suspect, the victim, object, or the crime scene. We report the use of nondestructive ATR-FTIR spectroscopy combined with chemometrics for the classification of 10 brands of lipsticks with nine samples each. Chemometric method of partial least square-discriminant analysis (PLS-DA) has been employed to interpret the data and classify the samples into their respective classes. The PLS-DA model provides an AUC figure above 0.99 in all brands except one; for which it is slightly less at 0.94. We have also tested the traces of these lipstick samples on different substrates treating them as unknowns in the already trained PLS-DA model. 100% of the samples on nine substrates viz. a cotton, nylon, plastic, dry tissue, denim (blue jeans), wet tissue, nitrile gloves, white paper, and polyester were correctly attributed to their source brand. In conclusion, the results suggest that ATR-FTIR combined with the chemometrics is a rapid, nondestructive, and accurate method for the discrimination and source attribution of lipstick. This study has potential for use in actual forensic casework conditions.
Daily exposure to toxic metals through urban road dust from industrial, commercial, heavy traffic, and residential areas in Petaling Jaya, Malaysia: a health risk assessment

Shabanda IS, Koki IB, Low KH, Zain SM, Khor SM, Abu Bakar NK

Environ Sci Pollut Res Int, 2019 Dec;26(36):37193-37211.
PMID: 31745807 DOI: 10.1007/s11356-019-06718-2

Human health is threatened by significant emissions of heavy metals into the urban environment due to various activities. Various studies describing health risk analyses on soil and dust have been conducted previously. However, there are limited studies that have been carried out regarding the potential health risk assessment of heavy metals in urban road dust of < 63-μm diameter, via incidental ingestion, dermal contact, and inhalation exposure routes by children and adults in developing countries. Therefore, this study evaluated the health risks of heavy metal exposure via ingestion, dermal contact, and inhalation of urban dust particles in Petaling Jaya, Malaysia. Heavy metals such as lead (Pb), chromium (Cr), zinc (Zn), copper (Cu), and manganese (Mn) were measured using dust samples obtained from industrial, high-traffic, commercial, and residential areas by using inductively coupled plasma mass spectrometry (ICP-MS). The principal component and hierarchical cluster analysis showed the dominance of these metal concentrations at sites associated with anthropogenic activities. This was suggestive of industrial, traffic emissions, atmospheric depositions, and wind as the significant contributors towards urban dust contamination in the study sites. Further exploratory analysis underlined Cr, Pb, Cu, and Zn as the most representative metals in the dust samples. In accommodating the uncertainties associated with health risk calculations and simulating the reasonable maximum exposure of these metals, the related health risks were estimated at the 75th and 95th percentiles. Furthermore, assessing the exposure to carcinogenic and non-carcinogenic metals in the dust revealed that ingestion was the primary route of consumption. Children who ingested dust particles in Petaling Jaya could be more vulnerable to carcinogenic and non-carcinogenic risks, but the exposure for both children and adults showed no potential health effects. Therefore, this study serves as an important premise for a review and reformation of the existing environmental quality standards for human health safety.

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