摘要
建立了同时检测鸡肉和鸡蛋中7种硝基咪唑类化合物(MNZ、RNZ、DMZ、SNZ、ORN、TNZ和IPZ),以及相应的3种羟基代谢物(MNZOH、HMMNI和IPZOH)的高效液相色谱-串联质谱法(HPLC-MS/MS)。样品用乙酸乙酯提取,正己烷除脂,SCX固相萃取柱净化。采用Waters C18柱(100 mm×2.1 mm,1.8μm)分离,以0.1%甲酸甲醇溶液-0.1%甲酸水溶液为流动相,质谱采用多反应监测(MRM)模式检测,内标法定量。硝基咪唑及其代谢物在0.5~40 ng/mL范围内线性良好,相关系数在0.9909~0.9991之间;方法的检测限是0.5~1.0μg/kg,定量限为1.0~2.0μg/kg。在添加水平1.0~10.0μg/kg的回收试验中,平均回收率为70.5%~112%,相对标准偏差为3.21%~14.6%。该方法简单,灵敏度高,特异性强,回收率高,可同时检测在鸡蛋和鸡肉中硝基咪唑及其代谢物残留。
In this work,we established a method for the determination of seven kinds of nitromidazole compounds(MNZ,RNZ,DMZ,SNZ,ORN,TNZ and IPZ)and three kinds of corresponding hydroxy metabolites(MNZOH,HMMNI and IPZOH)in chicken and egg matrix by high performance liquid chromatography coupled to electrospray tandem mass spectrometry(HPLC-ESI-MS/MS).The nitromidazoles and their metabolites of interest were extracted from tissues with ethyl acetate,and the crude extracts were subject to liquid-liquid partition with hexane followed by strong cation exchange solid phase extraction.By gradient elution with methanol and water(containing 0.1%formic acid,volume fraction)on Waters C18 column(100 mm×2.1 mm,1.8μm),the compounds were then detected by tandem mass spectrometry under multiple reaction monitoring mode using internal standard method.The results showed that the calibration curves of the nitromidazoles and their metabolites were linear in a certain concentration range(0.5-40 ng/mL)with correlation coefficients of 0.9909-0.9991.The limits of detection were 0.5-1.0μg/kg,and the limits of quantitation were 1.0-2.0μg/kg.The average recoveries at three spiked levels of 1.0-10.0μg/kg were between 70.5%-112%with relative standard deviations of 3.21%-14.6%.The results indicate that the methods is sensitive,simple and accurate to simultaneously determine seven kinds of nitromidazoles and three kinds of their metabolites in chicken and egg.
作者
张静
高玉时
周倩
马丽娜
陆俊贤
唐修君
万玉
杨星星
赵敏
ZHANG Jing;GAO Yushi;ZHOU Qian;MA Lina;LU Junxian;TANG Xiujun;WAN Yu;YANG Xingxing;ZHAO Min(Jiangsu Institute of Poultry Sciences,Yangzhou 223125)
出处
《分析科学学报》
CAS
CSCD
北大核心
2021年第2期217-222,共6页
Journal of Analytical Science
基金
江苏省现代农业重点及面上项目(No.BE2018363)
江苏省属公益类科研院所自主科研经费(No.BM2018026)
江苏现代农业产业技术体系建设专项资金(JATS[2020]359)
扬州市社会发展面上项目(No.YZ2020060)。