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鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备
引用本文:常平平,许春南,张立新,郝小妹,高兴,陈超.鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备[J].中国畜牧兽医,2015,42(9):2278-2285.
作者姓名:常平平  许春南  张立新  郝小妹  高兴  陈超
作者单位:1. 北京勤邦生物技术有限公司, 北京 102206;
2. 北京市优质农产品产销服务站, 北京 100101
基金项目:国家重大科学仪器设备开发专项"全自动化学发光免疫分析仪工程化开发及应用(2013YQ140371)
摘    要:本试验建立了一种超高效液相色谱-电喷雾串联质谱测定鸡肉中金刚烷胺的分析方法。以甲醇-1%三氯乙酸作提取剂,采用超声波辅助溶剂萃取法萃取鸡肉中金刚烷胺,萃取液用MCX固相萃取柱进行净化浓缩。以BEH C18色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对质谱和色谱条件、提取剂的种类、超声提取时间、固相萃取柱及洗脱液的种类进行了优化,在0.1~20.0 ng/mL范围内线性关系良好(r=0.9998)。样品在5.0、10.0 和20.0 μg/kg添加水平的回收率为89.7%~101.4%,相对标准偏差(RSD)小于7.0%;方法的检测限为0.07 μg/kg,定量限为0.23 μg/kg。本方法灵敏度高、准确度高,能满足公司及相应鸡肉行业的客户进行鸡肉中金刚烷胺残留量的快速、高灵敏检测分析。本试验还根据金刚烷胺在动物体内的代谢动力学成功制备了浓度为11.16和7.18 mg/kg的金刚烷胺阳性鸡肉样品,为研发金刚烷胺ELISA试剂盒提供了相应的阳性样品。

关 键 词:超高效液相色谱&mdash  电喷雾串联质谱  金刚烷胺  鸡肉  阳性样品  
收稿时间:2015-01-26

Establishment of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Determination Method of Amantadine in Chicken and Preparation of Positive Samples
CHANG Ping-ping,XU Chun-nan,ZHANG Li-xin,HAO Xiao-mei,GAO Xing,CHEN Chao.Establishment of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Determination Method of Amantadine in Chicken and Preparation of Positive Samples[J].China Animal Husbandry & Veterinary Medicine,2015,42(9):2278-2285.
Authors:CHANG Ping-ping  XU Chun-nan  ZHANG Li-xin  HAO Xiao-mei  GAO Xing  CHEN Chao
Institution:1. Beijing Kwinbon Biotechnology Co., Ltd., Beijing 102206, China;
2. Beijing Quality Agricultural Production and Marketing Service Station, Beijing 100101, China
Abstract:An ultra performance liquid chromatography (UPLC)-tandem mass spectrometry analysis method was established in this experiment for determination of amantadine in chicken.1% trichloroacetic acid with methanol as extraction liquid, the ultrasonic assisted solvent extraction was used to extract amantadine in chicken, extract liquid was purified and enriched in MCX solid-phase extraction column.Using C18 chromatographic column as separation column, in the positive ion mode, we detected the samples by electrospray ionization tandem mass spectrometry.Mass spectrometry and chromatographic conditions, the type of extract liquid, ultrasonic extraction time, the types of solid-phase extraction column and eluent were optimized.Under optimal conditions, a good linearity (r=0.9998) in the ranges of 0.1 to 20.0 ng/mL was obtained, the recoveries were 89.7% to 101.4% in the additive levels of 5.0, 10.0 and 20.0 μg/kg, the limit of detection (LOD) of amantadine was 0.07 μg/kg, the limit of quantiation (LOQ) of amantadine was 0.23 μg/kg, and the relative standard deviations (RSD) were below 7.0%.This novel approach had high sensitivity and accuracy, and was successfully applied to rapid and high sensitive detection of amantadine residues in chicken.The positive samples of amantadine in chicken were successfully prepared with concentrations of 11.16 and 7.18 mg/kg, which could be used for the research of ELISA kits of amantadine.
Keywords:ultra performance liquid chromatography-tandem mass spectrometry  amantadine  chicken  positive sample  
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