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| Simultaneous Determination of Mebendazole and Its Metabolites Residues in Fishery Products by High Performance Liquid Chromatography Tandem Mass Spectrometry with Isotope Dilution |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:Isotope dilution menbendazole hydroxy mebendazole amino menbendazole metabolites HPLC-MS/MS fishery products |
| Author | Institution |
| 刘永涛,艾晓辉,杨红 |
1.中国水产科学研究院长江水产研究所农业部淡水鱼类种质监督检验测试中心， 2.中国水产科学研究院淡水渔业研究中心 |
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| 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 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. |
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