Optimization of LC-MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges |
| |
Authors: | Soler Carla Hamilton Brett Furey Ambrose James Kevin J Mañes Jordi Picó Yolanda |
| |
Affiliation: | a Laboratori de Bromatologia i Toxicologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, València, Spain b PROTEOBIO Department of Chemistry, Mass Spectrometry Centre for Proteomics and Biotoxin Research, Cork Institute of Technology, Bishopstown, Cork, Ireland |
| |
Abstract: | This paper describes an analytical method involving a simple solvent extraction for the simultaneous liquid chromatography coupled to quadrupole tandem mass spectrometry (LC-MS/MS) determination of carbosulfan, its most toxic metabolite -carbofuran -, and its other main metabolites - 3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenolcarbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran and dibutylamine - in oranges. Chromatography was performed on a Zorbax Bonus-RP (150 mm × 2.1 mm, 5 μm). The mobile phase was a ternary gradient water-methanol-acetonitrile with 1.0 mM ammonium acetate at flow rate of 0.2 ml min−1. The LC separation and MS/MS optimization were studied to select the most appropriate operating conditions. The method developed has also been validated. The limits of quantification (LOQs) were from 1 μg kg−1 for carbofuran to 10 μg kg−1 for 3-keto-7-phenolcarbofuran. Extracts spiked with carbosulfan and its metabolites, at LOQ level, yielded average recoveries in the range 60-94%, with relative standard deviations (R.S.D.s) less than 15%. Calibration curves for carbosulfan and its metabolites (range LOQ-1000LOQ) were linear, with coefficients of correlations better than 0.990. The method was successfully applied to establish the primary degradation products in oranges treated with carbosulfan. The LC-MS/MS method developed is simple, rapid, and suitable for the quantification and confirmation of carbosulfan and seven of its main metabolites in orange at levels lower than 10 μg kg−1. |
| |
Keywords: | Liquid chromatography-tandem mass spectrometry Triple quadrupole Food Fruits Pesticides Metabolites Carbamates |
本文献已被 ScienceDirect PubMed 等数据库收录! |
|