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

作　　者：刘永涛[1,2] 艾晓辉[1,2] 杨红[1,2] 

机构地区：[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,湖北武汉430223 [2]中国水产科学研究院淡水渔业研究中心,江苏无锡214081

出　　处：《分析测试学报》2011年第6期640-645,共6页Journal of Instrumental Analysis

基　　金：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)

摘　　要：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氨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2mL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0．2mL／min，用配有加热电喷雾离子源的三重四极杆质谱进行选择反应离子监测。3种化合物在0．5～100μg／L范围内呈良好线性，相关系数均不低于0．9992。在草鱼、克氏原螯虾和甲鱼空白肌肉中加标水平为1～40μg/kg时，方法的回收率为91％-112％，相对标准偏差为1．5％～10．7％，检出限为0．5μg/kg，定量下限为1．0μg／kg。该方法灵敏度高，操作简便、准确、快速，适用于快速测定水产品中甲苯咪唑及其代谢物的残留量。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 mmi. 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 （ r^2 ） 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 aecu rate, and was suitable for the simultaneous qualitative and quantitative confirmations of menbendazole and 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 

分 类 号：O657.63[理学—分析化学] S482.3[理学—化学]