Dataset Information

Simultaneous determination of triazole fungicides in animal-origin food by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry.

ABSTRACT: A method for the simultaneous determination of 21 triazole fungicides in animal-origin foods was established by using UPLC-MS/MS. The dilution solvent, extraction solvent, and QuEChERS purification adsorbent composition, were optimized. The response value of the target compound was the highest and the chromatographic peak shape was optimal under the following conditions: water-acetonitrile as the mobile phase, acetonitrile to extract the target compound, C18 (100 mg) as the adsorbent, and water-acetonitrile as the diluent. Our method was validated under electrospray ionization (ESI) + conditions with six animal-origin foods. The 21 triazole fungicides showed good linear relationships (0.1-20 μg∙L^-1, R² > 0.99). The limits of detection and quantitation ranged from 0.1 to 0.3 μg∙kg^-1 and 0.3 to 0.9 μg∙kg^-1, respectively. The average recoveries ranged from 72.0% to 114.8% with RSDs < 9.9%. Therefore, our method was suitable for the determination of pesticide residues in commercially available animal-origin samples.

SUBMITTER: Xing L

PROVIDER: S-EPMC10740030 | biostudies-literature | 2023 Dec

REPOSITORIES: biostudies-literature

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Simultaneous determination of triazole fungicides in animal-origin food by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry.

Xing Lijie L Liu Yang Y Li Wenqi W Zou Liangjun L Wang Yuan Y Luo Ruifeng R

Food chemistry: X 20231021

A method for the simultaneous determination of 21 triazole fungicides in animal-origin foods was established by using UPLC-MS/MS. The dilution solvent, extraction solvent, and QuEChERS purification adsorbent composition, were optimized. The response value of the target compound was the highest and the chromatographic peak shape was optimal under the following conditions: water-acetonitrile as the mobile phase, acetonitrile to extract the target compound, C18 (100 mg) as the adsorbent, and water- ...[more]

PMID: 38144806

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Project description:Glyphosate is the most used herbicide in agriculture. Its major metabolite is AMPA (aminomethylphosphonic acid), but N-acetyl-AMPA and N-acetylglyphosate are also metabolites of interest. For risk assessment, a general residue definition was proposed as the sum of glyphosate, AMPA, N-acetyl-glyphosate and N-acetyl-AMPA, expressed as glyphosate. A confirmatory method for glyphosate in fat, liver and kidneys, as well as a confirmatory method for AMPA and N-acetyl-glyphosate in all matrices, are still missing. In this paper, we present a method for the quantitative determination of glyphosate residues and its metabolites AMPA, N-acetyl-AMPA and N-acetyl-glyphosate by liquid chromatography-mass spectrometry (LC-MS/MS) in adipose tissue, liver, eggs, milk and honey without derivatization. Different chromatographic columns were tested, with the Hypercarb column providing the best results. The analytes were eluted with mobile phases of acidified water with 1.2% formic acid and 0.5% formic acid in acetonitrile. Sample purification procedures were also optimized by varying the solvent extraction mixtures (water, methanol and mixture ψ (methanol, water) = 1:1, each with the addition of 1% formic acid (v/v)), using different sorbents in solid phase extraction (SPE) (polymeric cationic (PCX) and anionic (PAX)) and using dispersive solid phase extraction (dSPE) (C18 and PSA) by modifying the extraction procedures. Finally, the analytes were extracted from the samples with 1% formic acid in water (v/v). Milk and adipose tissue were purified by the addition of dichloromethane, while liver and egg samples were purified by SPE with a mixed cation exchange sorbent and ultrafiltration with cut-off filters. The proposed analytical procedures were validated according to SANTE/11312/2021 guidelines: linearity, limits of quantification, precision and accuracy were determined for all matrices. The limits of quantification (LOQs) ranged from 0.025 to 0.2 mg kg-1. Precision, expressed as relative standard deviation, was <20%, while accuracy, expressed as analytical recovery, ranged from 70% to 120%. During method validation, the measurement uncertainty was estimated to be <50% for all analytes. Good validation parameters according to the SANTE document were achieved for all analytes. Therefore, the method can be considered reliable and sensitive enough for routine monitoring of polar pesticides. The application of the accredited method in routine analysis will provide data that are useful for the re-evaluation of risk assessment studies in foods of animal origin.

Dataset Information

Simultaneous determination of triazole fungicides in animal-origin food by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry.

Publications

Simultaneous determination of triazole fungicides in animal-origin food by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry.

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