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A direct high-performance liquid chromatographic method for the determination of therminol 66 contamination in commercial glycerin and fatty acids

Moh MH, Tang TS, Tan GH

J Chromatogr Sci, 2001 Dec;39(12):508-12.
PMID: 11767238

A simple and sensitive high-performance liquid chromatographic method for the determination of Therminol 66 thermal heating fluid in glycerin and fatty acids is developed. Sample solutions dissolved in methanol-tetrahydrofuran (50:50, v/v) are injected directly into a reversed-phase C18 column and eluted with a methanol and water mixture (88:12, v/v). The concentration of the thermal heating fluid is monitored by fluorescence detection at 257 nm (excitation) and 320 nm (emission). The calibration graph obtained from various concentrations of the thermal heating fluid in the methanol and tetrahydrofuran mixture is linear (correlation coefficient = 0.999), and the limit of detection is 0.01 microg/mL. Spiked glycerin containing 0.1 to 1.0 microg/g of the thermal heating fluid also gives good linearity with a mean recovery of 95.3%. The mean intra- and interassay precision are 1.80-6.51% and 5.71-9.03%, respectively, at the 0.1-microg/g level. The method is simple and does not require any pretreatment step, thus it is ideal for quality assurance purposes.

Matched MeSH terms: Chromatography, High Pressure Liquid
Application of the artificial neural network in quantitative structure-gradient elution retention relationship of phenylthiocarbamyl amino acids derivatives

Tham SY, Agatonovic-Kustrin S

J Pharm Biomed Anal, 2002 May 15;28(3-4):581-90.
PMID: 12008137

Quantitative structure-retention relationship(QSRR) method was used to model reversed-phase high-performance liquid chromatography (RP-HPLC) separation of 18 selected amino acids. Retention data for phenylthiocarbamyl (PTC) amino acids derivatives were obtained using gradient elution on ODS column with mobile phase of varying acetonitrile, acetate buffer and containing 0.5 ml/l of triethylamine (TEA). Molecular structure of each amino acid was encoded with 36 calculated molecular descriptors. The correlation between the molecular descriptors and the retention time of the compounds in the calibration set was established using the genetic neural network method. A genetic algorithm (GA) was used to select important molecular descriptors and supervised artificial neural network (ANN) was used to correlate mobile phase composition and selected descriptors with the experimentally derived retention times. Retention time values were used as the network's output and calculated molecular descriptors and mobile phase composition as the inputs. The best model with five input descriptors was chosen, and the significance of the selected descriptors for amino acid separation was examined. Results confirmed the dominant role of the organic modifier in such chromatographic systems in addition to lipophilicity (log P) and molecular size and shape (topological indices) of investigated solutes.

Matched MeSH terms: Chromatography, High Pressure Liquid
Quantitative application of fecal sterols using gas chromatography-mass spectrometry to investigate fecal pollution in tropical waters: western Malaysia and Mekong Delta, Vietnam

Isobe KO, Tarao M, Zakaria MP, Chiem NH, Minh le Y, Takada H

Environ Sci Technol, 2002 Nov 1;36(21):4497-507.
PMID: 12433157

This is the first report on fecal pollution using molecular markers in Southeast Asia where serious sewage pollution has occurred. A simple and sensitive analytical method using gas chromatography-mass spectrometry for 10 sterols in various environmental samples was developed to monitor extensive areas of tropical Asia. First, the method was applied to wastewater to confirm that >95% of sterols existed in the particulate phase. Then the approach was applied to a tropical Asian region, Malaysia and Vietnam, with a selection of 59 sampling stations in total. River water and sediment samples were collected and analyzed for chemical markers (coprostanol and other sterols) and microbiological markers (fecal coliforms and fecal streptococci). Particulate coprostanol concentrations ranged from <0.0001 to 13.47 microg/L in tropical river and estuarine waters, indicating severe fecal pollution in populous areas. Coprostanol concentrations in the sediments ranged from 0.005 to 15.5 microg/g-dry. The sedimentary coprostanol concentrations were lower than those reported in some urban areas of industrialized countries. This is probably because frequent heavy rain induces intensive input of eroded soil, which dilutes fecal material in river sediments. The relationship between the concentrations of fecal sterols and bacterial indicators was examined in an attempt to develop public health criteria for coprostanol levels applicable to the tropical region. Coprostanol concentrations of 30-100 ng/L or percent coprostanol levels of 2% corresponded to approximately 1000 fecal coliforms per 100 mL, which is set for secondary contact limit in many countries. These coprostanol concentrations were lower than those proposed as criteria in temperate countries, probably owing to greater survival of bacteria in warmer tropical waters. On the basis of these criteria, extensive monitoring of sediments suggests that poor sanitary conditions exist in most of the urbanized area of Malaysia and in several urban and rural sites in Vietnam.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Distribution of oil and grease and petroleum hydrocarbons in the Straits of Johor, peninsular Malaysia

Abdullah AR, Woon WC, Bakar RA

Bull Environ Contam Toxicol, 1996 Jul;57(1):155-62.
PMID: 8661474
Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Comparison of solvent extraction and solid-phase extraction for the determination of organochlorine pesticide residues in water

Tan GH

Analyst, 1992 Jul;117(7):1129-32.
PMID: 1524230

Solid-phase extraction (SPE) of organochlorine pesticide residues from environmental water samples was evaluated using octadecyl (C18)-bonded porous silica. The efficiency of SPE of these pesticide residues from reagent water samples at 1-5 micrograms dm-3 levels was compared with those obtained by solvent extraction with hexane and Freon TF (trichlorotrifluoroethane). Average recoveries exceeding 80% for these organochlorine pesticides were obtained via the SPE method using small cartridges containing 100 mg of 40 microns C18-bonded porous silica. The average recovery by solvent extraction with hexane and Freon TF exceeded 90% in both instances. It was concluded that the recoveries and precision for the SPE of organochlorine pesticides were poorer than those for the solvent extraction method. Organochlorine pesticide residue levels in environmental water samples from two major rivers flowing through predominantly rice-growing areas were monitored by gas chromatography using the solvent extraction method with hexane. Exceptionally high levels of organochlorine pesticide residues such as BHC, DDT, heptachlor, endosulfan and dieldrin were found in these water samples.

Matched MeSH terms: Chromatography, Gas
Hydrocarbons in seawater and sediment from the west coast of Peninsular Malaysia

Abdullah AR, Tahir NM, Wei LK

Bull Environ Contam Toxicol, 1994 Oct;53(4):618-26.
PMID: 8000192
Matched MeSH terms: Chromatography, Gel
Fatty acid compositions in mucus and roe of Haruan, Channa striatus, for wound healing

Jais AM, Matori MF, Kittakoop P, Sowanborirux K

Gen. Pharmacol., 1998 Apr;30(4):561-3.
PMID: 9522175

1. Fatty acid profiles in the external mucus extract and roe of Channa striatus were determined using gas chromatography (GC). 2. The mucus samples were collected by inducing hypothermic stress (-20 degrees C) for about 1 hr, and the roe were collected from gravid females at night soon after they liberated their eggs in a spawning program. 3. All mucus and roe samples were freeze-dried, except a part of roe which was not. 4. The mucus extract contained unsaturated fatty acid (oleic acid, C18:1 and linoleic acid, C18:2) as a major component, 21.25% and 22.47% of total lipid. 5. For the freeze- and nonfreeze-dried roe, the major components of fatty acid were somewhat similar to the mucus but with higher percentages: 58.56%, 26.08% and 45.76%, 20.94%. Interestingly, the nonfreeze-dried roe contained a large proportion of arachidic acid, C20:0 (22.16%), which was totally absent in the freeze-dried roe samples. 6. This profiling of the fatty acid mucus extract and roe is useful in strengthening the earlier claims that haruan possesses a potential remedy for wound healing (Mat Jais et al., 1994). Therefore, we are discussing the possibility of getting an optimum amount of the essential fatty acid for wound healing from various other parts of the fish without sacrificing the fish.

Matched MeSH terms: Chromatography, Gas
Analysis of pesticide residues in Peninsular Malaysian waterways

Huat TG, Hock GS, Vijayaletchumy K

Environ Monit Assess, 1991 Oct;19(1-3):469-79.
PMID: 24233962 DOI: 10.1007/BF00401334

The use of organochlorine pesticides has caused concern due to their effects on human health and the Malaysian aquatic ecosystem, particularly so in view of their persistent and bioaccumulative properties. Since the extent of organochlorine pesticide pollution in Malaysian waterways is unknown except for isolated instances, a systematic survey has now been carried out. Water samples from various rivers were extracted, cleaned up with Florisil and analysed for the individual organochlorine pesticides by gas chromatography (GC) with an electron capture detector (ECD). DDE, DDT and heptachlor were present in all the river water samples of the west coast of Peninsular Malaysia. Other organochlorine pesticides were also identified from the water samples. However, the levels of all these are still below criteria values for Malaysian aquatic life, indicating that organochlorine pesticide pollution is less of a problem than other organic or inorganic pollutants.

Matched MeSH terms: Chromatography, Gas
Phenolic water pollutants in a Malaysian River basin

Abdullah P, Nainggolan H

Environ Monit Assess, 1991 Oct;19(1-3):423-31.
PMID: 24233958 DOI: 10.1007/BF00401330

Phenolic chemicals with their very low taste and odour thresholds, high persistence and toxicity, are of growing concern as water pollutants. The compounds are known to exist in raw water as well as in treated water. The level of phenolic priority pollutants in water within the catchment area of the Linggi River Treatment Plant in Negeri Sembilan, Malaysia, which includes the Linggi river basin, was monitored. The 4-aminoantipyrin colourimetric method was used to determine total phenols whereas capillary column gas chromatography was used to determine the individual compounds. The results show that at most sampling stations, particularly those within the Seremban municipality, the level of phenols was found to exceed the recommended Malaysian standard of 2.0 μg/L(-1) for raw water. This is seen as the direct impact of industrial and urbanization of the area and clearly indicates the unhealthy state of the Linggi river. The results also indicate the need to improve the water quality if the river is going to be used as a source of raw water.

Matched MeSH terms: Chromatography, Gas
Fulltext Cerebrospinal fluid lactic acid concentration in bacterial meningitis

Pit S, Jamal F, Isahak I, Minhaj AA

Med J Malaysia, 1987 Dec;42(4):302-5.
PMID: 3454403

Lactic acid concentration was determined in 37 specimens of cerebrospinal fluid by gas liquid chromatography. It was found to be raised (30 mg/dl) in 15 specimens from culture positive cases of bacterial meningitis and one of fungal meningitis. It was < 30 mg/dl in cerebrospinal fluid from four cases of viral meningoencephalitis and 10 contaminated specimens. It was also raised in two specimens from culture negative cases. Determination of cerebrospinal fluid lactic acid concentration by gas liquid chromatography provides a useful, additional test in the diagnosis of bacterial meningitis

Matched MeSH terms: Chromatography, Gas
An evaluation of TLC systems for opiate analysis

Rajananda V, Nair NK, Navaratnam V

Bull Narc, 1985 Jan-Mar;37(1):35-47.
PMID: 4063572

The authors selected 38 thin-layer-chromatography (TLC) systems described in the available literature published over the last 10 years and evaluated those systems with respect to their suitability for detection and identification of opiates in urine, opium and heroin, as well as adulterants in heroin. A total of 14 substances: 8 opiates (morphine, 6-monoacetylmorphine, diacetylmorphine, codeine, acetylcodeine, noscapine, papaverine and thebaine) and 6 adulterants (ephedrine, quinine, methadone, caffeine, cocaine and strychnine) were used as test samples for this research. Using laboratory-coated plates and pre-coated plates, 15 and 13 TLC systems, respectively, were found to be able to detect and identify morphine and codeine in urine without interference from the remaining 12 substances. For the detection of opiates in opium samples as well as opiates and adulterants in illicit heroin samples the TLC system: chloroform-n-hexane-triethylamine (9:9:4) which was developed by the National Drug Research Centre, Penang, Malaysia, was found to be most suitable on both laboratory-coated and pre-coated plates. In addition, the following two systems, one on laboratory-coated plates--hexane-chloroform-diethylamine (50:30:7)--and the other on pre-coated plates--benzene-dioxane-ethanol-ammonia (50:40:5:5; T-7)--were also found to be among most suitable TLC systems for the analysis of opiates in opium samples. The article also presents the relative cost of each of the 38 evaluated TLC systems.

Matched MeSH terms: Chromatography, Thin Layer
Leaching of bisphenol A from new and old babies' bottles, and new babies' feeding teats

Tan BL, Mustafa AM

Asia Pac J Public Health, 2003;15(2):118-23.
PMID: 15038686

Bisphenol A is the monomer used in the manufacture of polycarbonate. Bisphenol A is also known to mimic the female hormone estrogen. In this study, the possibility of the leaching of bisphenol A from polycarbonate babies' bottles and feeding teats was investigated. Bisphenol A was extracted from water samples exposed to the bottles and teats using liquid-liquid extraction. Bisphenol A was analysed by gas chromatograph-mass spectrometer with quadrapole detector in selected ion monitoring mode. Mean leaching of bisphenol A from 100 used babies' bottles when filled with water at 25 degrees C and 80 degrees C were 0.71 +/- 1.65 ng/cm2 (mean +/- standard deviation) and 3.37 +/- 5.68 ng/cm2 respectively. Mean leaching of bisphenol A from 30 new babies' bottles when filled with water at 25 degrees C and 80 degrees C were 0.03 +/- 0.02 ng/cm2 and 0.18 degrees 0.30 ng/cm2 respectively. Bisphenol A was observed to have leached from babies' feeding teats into 37 degrees C water ranged from non-detectable to 22.86 ng/g. The technique employed in this study is fast, reliable and economical.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Homocystinuria-a case report

Peng LH, Perumal R

Med J Malaysia, 1976 Mar;30(3):213-9.
PMID: 985681
Matched MeSH terms: Chromatography
Fulltext Reinventing nano drug delivery systems for hydrophilic active ingredients in Ayurvedic lipid based formulations containing poly herbal decoction

Duraipandi S, Selvakumar V

J Ayurveda Integr Med, 2019 01 08;11(3):224-227.
PMID: 30635246 DOI: 10.1016/j.jaim.2018.01.008

BACKGROUND: Anu Tailam, an Ayurvedic medicated oil where 'anu' meant for atom and 'tailam' meant for oil and virtually meant for 'oil of subtle or atomic size particles'. Since the major active ingredients in this formulation are incorporated from the polyherbal decoction, it is expected to contain predominantly water soluble ingredients.
OBJECTIVES: It is hypothesized that these polar active botanical ingredients are present in the formulation should be either suspended in the form of submicron particles or entrapped in the submicron vesicular structures since the formulation did not show any precipitation or phase separation instead showed a monophasic oily liquid with very little moisture.
MATERIALS AND METHODS: In the present investigation, the micro architecture of the anu tailam is studied via column chromatography and high performance thin layer chromatography to prove the contents are polar hydrophilic compounds followed by optical microscopy, photon correlation Spectroscopy (PCS) and environmental scanning electron microscope (ESEM) to study the particle/vesicle size of the formulation.
RESULTS: In this study, it was proved that the formulation contained only polar ingredients and can be extracted in polar solvents like methanol and ethanol. It was also found that the formulation taken for study contained nano particles of the active botanical ingredients embedded in a network of vesicular structures of the lipid base.
CONCLUSION: The selected Ayurvedic formulation 'anutailam' found to contain novel nano drug delivery system to deliver water soluble ingredients across barriers.

Matched MeSH terms: Chromatography, Thin Layer
Fulltext Optimization of headspace solid phase microextraction (HS-SPME) for the extraction of volatile organic compounds (VOCs) in MD2 pineapple

Syaidatul Faraha Zainuddin, Siti Raihan Zakaria, Norashikin Saim, Rossuriati Dol Hamid, Rozita Osman

Science Letters, 2020;14(2):58-70.
MyJurnal

Headspace solid phase microextraction (HS-SPME) was employed for the extraction of volatile organic compounds (VOCs) in MD2 pineapple (Ananas comosus L. var. comosus cv. MD2). Optimisation of HS-SPME operating parameters was conducted using three-factor, three-level Box–Behnken response surface experimental design to evaluate the interactive effects of temperature (30 – 50 ºC), extraction time (10 – 30 min) and salting effect (1 – 3 g of salt addition) on the amount of selected VOCs. Determination of VOCs was done using gas chromatography with spectrometry detector (GC-MSD). Extraction temperature was found to be significant (p < 0.05) in increasing the amount of selected VOCs (ethyl acetate, methyl isobutyrate and butanoic acid methyl ester). Based on the maximum amount of these VOCs, the optimum operating extraction conditions for HS-SPME were set up at temperature of 30 °C, time of 29 min and salt addition of 1 g. The optimized HS-SPME conditions were employed for the extraction of VOCs from pineapple of different varieties.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fulltext Inhibition of Quorum Sensing and Biofilm Formation in Chromobacterium violaceum by Fruit Extracts of Passiflora edulis

Venkatramanan M, Sankar Ganesh P, Senthil R, Akshay J, Veera Ravi A, Langeswaran K, et al.

ACS Omega, 2020 Oct 13;5(40):25605-25616.
PMID: 33073086 DOI: 10.1021/acsomega.0c02483

Chromobacterium violaceum (C. violaceum) is a Gram-negative, rod-shaped facultatively anaerobic bacterium implicated with recalcitrant human infections. Here, we evaluated the anti-QS and antibiofilm activities of ethyl acetate extracts of Passiflora edulis (P. edulis) on the likely inactivation of acyl-homoserine lactone (AHL)-regulated molecules in C. violaceum both by in vitro and in silico analyses. Our investigations showed that the sub-MIC levels were 2, 1, and 0.5 mg/mL, and the concentrations showed a marked reduction in violacein pigment production by 75.8, 64.6, and 35.2%. AHL quantification showed 72.5, 52.2, and 35.9% inhibitions, inhibitions of EPS production (72.8, 36.5, and 25.9%), and reductions in biofilm formation (90.7, 69.4, and 51.8%) as compared to a control. Light microscopy and CLSM analysis revealed dramatic reduction in the treated biofilm group as compared to the control. GC-MS analysis showed 20 major peaks whose chemical structures were docked as the CviR ligand. The highest docking score was observed for hexadecanoic acid, 2-hydroxy-1-(hydroxymethyl) ethyl ester bonds in the active site of CviR with a binding energy of -8.825 kcal/mol. Together, we found that hexadecanoic acid, 2-hydroxy-1-(hydroxymethyl) ethyl ester remarkably interacted with CviR to inhibit the QS system. Hence, we concluded that hexadecanoic acid, 2-hydroxy-1-(hydroxymethyl) ethyl ester of P. edulis could likely be evaluated for treating C. violaceum infections.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fulltext Dual bioactivities of laurus nobilis essential oil

Nur Afiqah Saparin, Mohd Muzamir Mahat, Muhd Fauzi Safian, Shahrul Hisham Zainal Ariffin, Nor Azah Mohamad Ali, Zaidah Zainal Ariffin

Science Letters, 2020;14(1):62-67.
MyJurnal

The evolution of cosmetic products results in the growing demands for cosmetics that are preservatives free. Plant essential oils were found to be a promising antimicrobial and also antioxidant agent. In this study, Cymbopogon citratus (lemongrass), Laurus nobilis (bay leaf) and Backhousia citriodora (lemon myrtle) essential oils were selected and evaluated for their antimicrobial properties. It was found that Laurus nobilis exhibited strong antimicrobial activity against the selected bacteria Streptococcus saprophyticus (ATCC 49619), Streptococcus aureus (ATCC 22923), Streptococcus pyogenes (ATCC 29436), Pseudomonas aeruginosa (ATCC 13048), Klebsiella pneumoniae (ATCC 700603), Escherichia coli (ATCC 22922) with MIC ranging between 7.8 ug/mL to 250 μg/mL. The antioxidant activity of selected essential oils was determined by antioxidant assays which were 1,1-Diphenyl-2-picrylhydrazyl assay (DPPH), determination of ferric reducing antioxidant power assay (FRAP) and β-Carotene/linoleic acid bleaching assay. Backhousia citriodora and Laurus nobilis showed the highest antioxidant activity.
n-Octanal and β-Selinene were identified to be the major components with peak area of 26.37 % and 13.92 % respectively in secondary metabolites analysis by Gas Chromatography-Mass Spectrometry (GCMS).

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fulltext Microbial Biodegradation of Paraffin Wax in Malaysian Crude Oil Mediated by Degradative Enzymes

Adlan NA, Sabri S, Masomian M, Ali MSM, Rahman RNZRA

Front Microbiol, 2020;11:565608.
PMID: 33013795 DOI: 10.3389/fmicb.2020.565608

The deposition of paraffin wax in crude oil is a problem faced by the oil and gas industry during extraction, transportation, and refining of crude oil. Most of the commercialized chemical additives to prevent wax are expensive and toxic. As an environmentally friendly alternative, this study aims to find a novel thermophilic bacterial strain capable of degrading paraffin wax in crude oil to control wax deposition. To achieve this, the biodegradation of crude oil paraffin wax by 11 bacteria isolated from seawater and oil-contaminated soil samples was investigated at 70°C. The bacteria were identified as Geobacillus kaustophilus N3A7, NFA23, DFY1, Geobacillus jurassicus MK7, Geobacillus thermocatenulatus T7, Parageobacillus caldoxylosilyticus DFY3 and AZ72, Anoxybacillus geothermalis D9, Geobacillus stearothermophilus SA36, AD11, and AD24. The GCMS analysis showed that strains N3A7, MK7, DFY1, AD11, and AD24 achieved more than 70% biodegradation efficiency of crude oil in a short period (3 days). Notably, most of the strains could completely degrade C37-C40 and increase the ratio of C14-C18, especially during the initial 2 days incubation. In addition, the degradation of crude oil also resulted in changes in the pH of the medium. The degradation of crude oil is associated with the production of degradative enzymes such as alkane monooxygenase, alcohol dehydrogenase, lipase, and esterase. Among the 11 strains, the highest activities of alkane monooxygenase were recorded in strain AD24. A comparatively higher overall alcohol dehydrogenase, lipase, and esterase activities were observed in strains N3A7, MK7, DFY1, AD11, and AD24. Thus, there is a potential to use these strains in oil reservoirs, crude oil processing, and recovery to control wax deposition. Their ability to withstand high temperature and produce degradative enzymes for long-chain hydrocarbon degradation led to an increase in the short-chain hydrocarbon ratio, and subsequently, improving the quality of the oil.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry
Fulltext Biochemical Constituent of Ginkgo biloba (Seed) 80% Methanol Extract Inhibits Cholinesterase Enzymes in Javanese Medaka (Oryzias javanicus) Model

Hassan I, Wan Ibrahim WN, Yusuf FM, Ahmad SA, Ahmad S

J Toxicol, 2020;2020:8815313.
PMID: 33029137 DOI: 10.1155/2020/8815313

Background: Pathophysiological changes leading to the death of nerve cells present in the brain and spinal cord are referred to as neurodegenerative diseases. Presently, treatment of these diseases is not effective and encounters many challenges due to the cost of drug and side effects. Thus, the search for the alternative agents to replace synthetic drugs is in high demand. Therefore, the aim of this study is to evaluate the anticholinesterase properties of Ginkgo biloba seed.
Methods: The seed was extracted with 80% methanol. Toxicity studies and evaluation of anticholinesterase activities were carried out in adult Javanese medaka (Oryzias javanicus). Phytochemical study to identify the bioactive lead constituents of the crude extract was also carried out using high performance liquid chromatography (HPLC).
Results: The result shows activities with high significant differences at P < 0.001 between the treated and nontreated groups. A bioactive compound (vitaxin) was identified with the aid of HPLC method.
Conclusion: The presence of bioactive compound vitaxin is among the major secondary metabolites that contribute to increasing activities of this plant extract. High anticholinesterase activities and low toxicity effect of this plant show its benefit to be used as natural medicine or supplements.

Matched MeSH terms: Chromatography, High Pressure Liquid
High Throughput Residue Analysis of Indaziflam and its Metabolites in Palm Oil Using Liquid Chromatography-Tandem Mass Spectrometry

Halim N, Kuntom A, Shinde R, Banerjee K

J AOAC Int, 2020 Sep 01;103(5):1237-1242.
PMID: 33241391 DOI: 10.1093/jaoacint/qsaa041

BACKGROUND: Indaziflam (IND) is a herbicide that is used in palm oil plantations for broad spectrum management of weeds. Until now, no validated method has been available for residue estimation of this herbicide in palm oil products.
OBJECTIVE: In this study, we report a rapid method for the residue analysis of IND and its metabolites, viz., IND-carboxylic acid, diaminotriazine, and triazine indanone in a wide range of palm oil matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS).
METHOD: The optimized sample preparation workflows included two options: (1) acetonitrile extraction (QuEChERS workflow), followed by freezing at -80°C and (2) acetonitrile extraction, followed by cleanup through a C18 solid phase extraction (SPE) cartridge. The optimized LC runtime was 7 min. All these analytes were estimated by LC-MS/MS multiple reaction monitoring.
RESULTS: Both sample preparation methods provided similar method performance and acceptable results. The limit of quantification (LOQ) of IND, IND-carboxylic acid, and triazine indanone was 0.001 mg/kg. For diaminotriazine, the LOQ was 0.005 mg/kg. The method accuracy and precision complied with the SANTE/12682/2019 guidelines of analytical quality control.
CONCLUSIONS: The potentiality of the method lies in a high throughput analysis of IND and its metabolites in a single chromatographic run with high selectivity and sensitivity. Considering its fit-for-purpose performance, the method can be implemented in regulatory testing of IND residues in a wide range of palm oil matrices that are consumed and traded worldwide.
HIGHLIGHTS: This work has provided a validated method for simultaneous residue analysis of indaziflam and its metabolites in crude palm oil and its derived matrices with high sensitivity, selectivity, and throughput.

Matched MeSH terms: Chromatography, Liquid

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