超高效液相色谱-串联质谱法同时测定鸡肉和鸡蛋中25种兽药残留  

Simultaneous Determination of Multiple Veterinary Medicine Residues in Chicken and Eggs by UHPLC-MS/MS

作　　者：陈兴连[1] 李倩 王志飞 方海仙[1] 李彦刚[1] 李茂宣 邵金良[1] CHEN Xing-lian;LI Qian;WANG Zhi-fei;FANG Hai-xian;LI Yan-gang;LI Mao-xuan;SHAO Jin-liang(Supervision&Testing Center for Farm Products Quality,Ministry of Rural Agriculture(Kunming Section),Quality Standardizing and Testing Technology Institute,Yunnan Academy of Agricultural Sciences,Kunming 650205,China;Yunnan Academy of Fishery Sciences,Kunming 650051,China)

机构地区：[1]云南省农业科学院质量标准与检测技术研究所,农业农村部农产品质量监督检验测试中心(昆明),云南昆明650205 [2]云南省渔业科学院,云南昆明650051

出　　处：《质谱学报》2021年第6期1046-1058,共13页Journal of Chinese Mass Spectrometry Society

基　　金：农业联合青年项目(2018FG 001-100);云南省科技厅科技计划项目(重大专项计划)(2018BC005-04);农产品绿色生产及质量安全控制关键技术研究与示范应用(重大科技专项)(202002AE320005)。

摘　　要：建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)法结合改良QuEChERS净化技术同时测定鸡肉和鸡蛋中25种兽药(磺胺类、喹诺酮类、氯霉素类、金刚烷胺类)残留。样品经稀盐酸水解、乙腈提取,向提取液中加入氯化钠盐析,乙腈和水相分层后,取出乙腈,经正己烷-环己烷溶液(1∶1,V/V)除脂、浓缩至干后,加0.2%甲酸-乙酸乙酯溶解残留物,过滤去除氯化钠,滤液再次浓缩近干,加入0.2%甲酸-甲醇后,以30 mg C18和60 mg PSA混合吸附剂净化。目标物经ZORBAX C18色谱柱(50 mm×2.1 mm×1.8μm)分离,正、负离子多反应监测模式同时采集,同位素内标法定量。结果表明,25种兽药在0.2~250μg/L范围内线性关系良好,线性相关系数r>0.99,方法检出限为0.1~0.9μg/kg,定量限为0.3~3.0μg/kg,在约1倍、5倍、20倍定量限添加水平下的平均回收率为79.5%~119%,相对标准偏差为0.9%~9.2%。本方法简便、准确、灵敏、经济,适用于鸡蛋和鸡肉中多类兽药残留的同时测定。A method of ultra high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)combined with modified QuEChERS purification technology was developed for the simultaneous determination of 25 veterinary medicine residues including four classes(sulfonamides,quinolones,chloramphenicols and amantidines)in chicken and egg.The samples were hydrolyzed by dilute hydrochloric acid,extracted by acetonitrile.Sodium chloride was added into the extracting solution to salt out.The acetonitrile was took out and degreased by n-hexane-cyclohexane solution(1∶1,V/V)after stratification of acetonitrile and aqueous phase and concentrated to dry.The residues were dissolved with 0.2%formic acid-ethyl acetate to remove the sodium chloride by filtrating and the filtrate was concentrated to dry again,then the sample was purified with a mixture of 30 mg of C18 and 60 mg PSA after adding 0.2%formic acid-methanol.The target compounds were separated by ZORBAX C18 chromatography column(50 mm×2.1 mm×1.8μm),the mass spectrometer data were acquired under multiple reaction monitoring(MRM)of positive and negative modes at the same time,and the residues were quantitated by isotope internal standard method.The results showed that the linear of 25 veterinary medicines is good in the range of 0.2-250μg/L.The linear correlation coefficients are more than 0.99,and the detection limits are in the range of 0.1-0.9μg/kg.The limits of quantification are 0.3-3.0μg/kg.The average recoveries at three spiked levels(about 1,5 and 20 folds of quantitative limits)are 79.5%-119%with the relative standard deviations of 0.9%-9.2%.The method is rapid,simple,accurate,sensitive and cheap,which is suitable for simultaneous determination of multiple vererinary medicine residues in eggs and chicken.

关 键 词：改良QuEChERS净化技术 超高效液相色谱-串联质谱(UHPLC-MS/MS) 鸡蛋 鸡肉 兽药 残留 

分 类 号：O657.63[理学—分析化学]