分析测试学报2011，Vol.30Issue(6)：640-645,6.DOI:10.3969/j.issn.1004-4957.2001.06.009
同位素稀释高效液相色谱-串联质谱法测定水产品中甲苯咪唑及其代谢物的残留量
Simultaneous Determination of Mebendazole and Its Metabolites Residues in Fishery Products by High Performance Liquid Chromatography Tandem Mass Spectrometry with Isotope Dilution
摘要
Abstract
A rapid method of liquid chromatography tandem mass spectrometric( HPLC -ESI MS/MS) with isotope dilution was developed for the simultaneous determination of residual mebendazole (MBZ) and its metabolites e.g. hydroxy-mebendazole ( MBZ - OH ) and amino-menbendazole ( MBZ - NH2 ) in fishery products. The sample, after adding disodium phosphate, was extracted with ethyl acetate. The extract was evaporated to dryness under nitrogen, and redissolved in 2 mL methanol -0. 1％ formic acid( 1: 1, by volume). The solution was defatted with n-hexane. The targeted compouds were seperated on Hypersil GOLD C18 column( 100 mm ×2. 1 mm i. d. , 3 tμm) using methanol -0. 1％ formic acid as mobile phase at a flow rate of 0. 2 mL/min, and analyzed by a triple quadrupole tandem mass spectrometer with a heated electrospray ionization source(HESI) and selected reaction monitoring(SRM). The standard curves were linear in the range of 0. 5 -100 μg/L for three analyzed drugs with correlation coefficient (r2 ) not less than 0. 999 2. At spiked levels of 1 -40 μg/kg in grass carp, crayfish and soft shelled turtle blank muscle sample, the average recoveries of MBZ, MBZ - OH and MBZ - NH2 ranged from 91％ to 112％ with their relative standard deviations(RSDs) of 1.5％ - 10. 7％. The detection limits for all the target compounds were 0. 5 μg/kg and the quantitation limits were 1.0 μμg/kg. The results showed that the method was simple, sensitive and accurate, and was suitable for the simultaneous qualitative and quantitative confirmations of menbendazoleand its metabolites residues in fishery products.关键词
同位素稀释/甲苯咪唑/羟基甲苯咪唑/氨基甲苯咪唑/代谢物/高效液相色谱-串联质谱法/水产品Key words
isotope dilution/ menbendazole/ hydroxy-mebendazole/ amino-menbendazole/ metab-olites/ HPLC - MS/MS/ fishery products分类
化学化工引用本文复制引用
刘永涛,艾晓辉,杨红..同位素稀释高效液相色谱-串联质谱法测定水产品中甲苯咪唑及其代谢物的残留量[J].分析测试学报,2011,30(6):640-645,6.基金项目
农业行业标准制定项目资助 （）
中央级公益性科研院所基本科研业务费专项资金资助项目(2011JBFA19) （2011JBFA19）
