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

建立了同时分析水产品中甲苯咪唑及其代谢物羟基甲苯咪唑和氮基甲苯咪唑的同位素稀释高效液相色谱串联质谱法.向样品中添加磷酸二氢钠溶液后用乙酸乙酯提取,提取液用氮气吹干后经2 mL甲醇-0.1%甲酸溶液(体积比1:1)溶解,正己烷去脂.以Hypersil GOLD为色谱分离柱,甲醇-0.1%甲酸溶液为流动相,流速为0.2 m...

Simultaneous Determination of Mebendazole and Its Metabolites Residues in Fishery Products by High Performance Liquid Chromatography Tandem Mass Spectrometry with Isotope Dilution

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 μm) 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 μg/kg.The results showed that the method was simple,sensitive and accu-rate,and was suitable for the simultaneous qualitative and quantitative confirmations of menbendazole and its metabolites residues in fishery products.