摘要
建立了高效液相色谱-串联质谱同时测定猪肉中29种咪唑类药物及其代谢物残留的检测方法。样品采用乙酸乙酯提取,浓缩复溶后加入乙腈饱和正己烷净化除脂,以0.3%(体积分数)甲酸水溶液和乙腈为流动相,反相C_(18)色谱柱梯度洗脱分离,采用电喷雾正离子(ESI+)源多反应监测(MRM)模式进行检测。29种化合物在0.05~20.0μg/L范围内线性关系良好,相关系数r^2>0.99。在1.0~5.0μg/kg添加范围内,平均回收率为65.4%~103%,相对标准偏差(RSD)为1.3%~6.8%。方法检出限为0.02~0.3μg/kg,定量限为0.1~1μg/kg。该方法简便、快速、灵敏,适用于猪肉中咪唑类及其代谢物残留的检测。
A method for the determination of29imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry has been developed.The samples were extracted with ethyl acetate,and then defatted with n-hexane after concentration of the extracts.The analytes were separated on a C,8reversed-phase column with0.3%(v/v)formic acid aqueous solution and acetonitrile as mobile phases,and finally analyzed using electrospray ionization in positive ion mode(ESI+)with multiple reaction monitoring(MRM).The linear ranges of the29compounds were from0.05to20.0pg/L with the correlation coefficients(r2)more than0.99.The average recoveries and relative standard deviations were65.4%-103%and1.3%-6.8%respectively in the spiked ranges of1.0-5.0pg/kg.The limits of detection and the limits of quantification were0.02-0.3pg/kg and0.1-1pg/kg respectively for the29imidazoles.The method is simple,rapid and sensitive.It is suitable for the detection of imidazoles and their metabolites in pork.
作者
杨旺火
吴少明
蔡小明
冯丽凤
陈言凯
李燕平
梁敏
YANG Wanghuo;WU Shaoming;CAI Xiaoming;FENG Lifeng;CHEN Yankai;LI Yanping;LIANG Min(National Quality Supervision and Testing Center for Processed Food,Fujian Inspection and Research Institute for Product Quality,Fuzhou 350002,China)
出处
《色谱》
CAS
CSCD
北大核心
2017年第10期1062-1067,共6页
Chinese Journal of Chromatography
关键词
液相色谱-串联质谱
咪唑类药物
残留
猪肉
liquid chromatography-tandem mass spectrometry (LC-MS/MS)
imidazoles
residue
pork
作者简介
通讯联系人.Tel:(0591)83762015,E-mail:wujifeijmshuywh@126.com.
