高效液相色谱-串联质谱快速测定饲料中硝基咪唑类药物及其代谢物残留  

Rapid Determination of Nitroimidazoles and Their Metabolites Residues in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：魏云计[1] 朱臻怡[1] 冯民[1] 何健[1] 沈金荣[1] 何正和 秦娴[1] 张伶俐[1] 钱怡平[1] 丁涛[2] WEI Yun-ji ZHU Zhen-yi FENG Min HE Jian SHEN Jin-rong HE Zheng-he QIN Xian ZHANG Ling-li QIAN Yi-ping DING Tao(State Key Laboratory of Feed Safety Testing（ Huaian）, Huaian Entry- Exit Inspection and Quarantine Bureau, Huaian 223001, China Animal, Plant and Food Inspection Center（APFIC） of Jiangsu Entry- Exit Inspection and Quarantine Bureau, Nanjing 210001, China)

机构地区：[1]淮安出入境检验检疫局国家饲料安全检测重点实验室(淮安),江苏淮安223001 [2]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001

出　　处：《分析测试学报》2017年第3期377-381,共5页Journal of Instrumental Analysis

基　　金：质检总局科技计划项目(2015IK131)

摘　　要：建立了高效液相色谱-串联质谱快速测定饲料中甲硝唑(MNZ)、甲硝唑代谢物(MNZOH)、二甲硝咪唑(DMZ)、二甲硝咪唑代谢物(HMMNI)、洛硝哒唑(RNZ)、异丙硝唑(IPZ)、异丙硝唑代谢物(IPZOH)残留的分析方法。样品经0.1 mol/L pH 8.0磷酸盐缓冲液和乙酸乙酯-丙酮(70∶30)提取,提取液经分散型固相萃取填料N-丙基乙二胺(PSA)净化后,再经正己烷脱脂,液-液分配净化,采用电喷雾电离源(ESI)正离子多反应监测(MRM)模式检测,氘代同位素内标法定量。该方法省去耗时的固相萃取过程,快速、简单、高效,7种目标分析物在2.0~100.0μg/L范围内线性关系良好,相关系数大于0.99,在5.0~25.0μg/kg范围内,3个加标水平的回收率为72.4%~95.6%,相对标准偏差(RSD)均小于12.5%;检出限为2.5μg/kg,定量下限为5.0μg/kg。A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method was developed for the rapid determination of metronidazole（MNZ）,metronidazole-OH（MNZOH）,dimetridazole（DMZ）,hydroxydimetridazole（HMMNI）,ronidazole（RNZ）,ipronidazole（IPZ）,ipronidazole-OH（IPZOH） residues in feed.The samples were extracted with 0.1 mol/L pH 8.0 phosphate buffer and ethyl acetate-acetone（70∶30,by volume）,then cleaned up with matrix solid phase dispersant primary secondary amine（PSA）.The extracts were defatted with hexane and cleaned up by liquid-liquid partition.The target compounds were detected by electrospray ionization（ESI） in positive mode using multiple reaction monitoring,and quantified by the isotope internal standard method.No solid phase extract（SPE） procedure was adopted,which made sample preparation simple and efficient.The calibration curves for seven target compounds were linear in the range of 2.0-100.0 μg/L with correlation coefficients more than 0.99.Average recoveries at spiked levels of 5.0-25.0 μg/kg were between 72.4% and 95.6%,with relative standard deviation less than 12.5%.The limits of detection（LOD） were 2.5 μg/kg,and the limits of quantitation（LOQ） were 5.0 μg/kg.

关 键 词：高效液相色谱-串联质谱 饲料 硝基咪唑类 代谢物 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]