超高效液相色谱-串联质谱法同时测定动物源性食品中9种多肽类抗生素残留  

Determination of Nine Polypeptide Antibiotics Residues in Animal Tissue Food by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：李莲微 杨晓聪 姚闽娜[1] 刘正才 李小晶 LI Lianwei;YANG Xiaocong;YAO Minna;LIU Zhengcai;LI Xiaojing(Food Science College of Fujian Agriculture and Forestry University,Fuzhou 350002,China;Food College of Xinyang College of Agriculture and Forestry,Xinyang 464000,China;Technology Center of Fuzhou Customs District,Fuzhou 350001,China)

机构地区：[1]福建农林大学食品科学学院,福建福州350002 [2]信阳农林学院食品学院,河南信阳464000 [3]福州海关技术中心,福建福州350001

出　　处：《食品工业科技》2022年第17期330-337,共8页Science and Technology of Food Industry

基　　金：福建农林大学科技创新专项基金项目(CXZX2017013);海关总署科研项目(2019HK106)。

摘　　要：建立了动物组织中9种多肽类抗生素残留的固相萃取-超高效液相色谱串联质谱(UPLC-MS/MS)检测方法。样品经甲醇-0.1 mol/L盐酸(7:3,v/v)混合溶剂提取,酸性氧化铝除杂、正己烷去除油脂,亲水-亲脂平衡(hydrophilic-lipophilic balance,HLB)固相萃取柱净化,以0.2%的甲酸水溶液和乙腈为流动相,经过C_(8)色谱柱(100A,150 mm×2 mm,3μm)梯度洗脱分离,使用电喷雾正离子化和多反应监测模式检测。结果表明,万古霉素和去甲万古霉素、恩拉霉素A、恩拉霉素B、太古霉素在2~200μg/L范围内,粘杆菌素A、粘杆菌素B、杆菌肽A在5~500μg/L范围内,维吉尼霉素M1在0.1~20μg/L范围内,各化合物定量离子的峰面积和样品质量浓度之间呈现良好的线性关系(R^(2)>0.99),方法的定量限(S/N=10)为1~20μg/kg,检出限为0.3~6μg/kg;以鸡肉、猪肉、猪肝、猪肾为基质,在加标水平为1~200μg/kg时,各个化合物的平均加标回收率为74.2%~96.3%,相对标准偏差为4.3%~14.6%。该方法简便、灵敏、准确,可用于动物组织中多肽类抗生素残留的同时测定。A method combining SPE and Ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS-MS) was developed for the simultaneous determination of nine polypeptide antibiotics in animal tissues.The samples were extracted by methanol and 0.1 mol/L hydrochloric acid(7:3,v/v),then cleaned with Alumina-A and nhexane,and finally purified by hydrophilic-lipophilic balance(hydrophilic-lipophilic balance,HLB) cartridge.The separations were performed on a C_(8)column(100A,150 mm×2 mm,3 μm) using a mobile phase gradient with 0.2% formic acid and acetonitrile.Electrospray positive ionization and multi-reaction monitoring(MRM) mode were used for detection.The calibration curves for vancomycin,norvancomycin,enramycin A,enramycin B,and teicoplanin,(concentration range 2~200 μg/L),colistin A,colistin B and bacitracin A(concentration range 5~500 μg/L),virginiamycin M1(concentration range 0.1~20 μg/L) were linear with correlation coefficients more than 0.99.The limits of quantification(LOQ,S/N=10) of 9 kinds of polypeptide antibiotics were varied from 1 μg/kg to 20 μg/kg,the detection limit of the method was 0.3 μg/kg to 6 μg/kg.The recovery experiments were performed with chicken,pork,liver and kidney samples spiked in the range of 1~200 μg/kg.The average recoveries ranged from 74.2% and 96.3% with the relative standard deviations(RSDs) of 4.3%~14.6%(n=6).The method is simple and rapid with high sensitivity and good reproducibility.Furthermore,this method is effective for the safety monitoring of polypeptide antibiotic residues in animal tissues.

关 键 词：多肽类抗生素 动物组织 固相萃取 超高效液相色谱串联质谱 

分 类 号：O657.63[理学—分析化学]