液相色谱-串联质谱测定豆芽中4种四环素类药物残留量研究  

Determination of Four Tetracycline Antibiotics in Bean Sprouts by HPLC-MS/MS

作　　者：韦航 邹强 李军法 荣杰峰 翁城武 许彩霞 高功敏 WEI Hang;ZOU Qiang;LI Jun-fa;RONG Jie-feng;WENG Cheng-wu;XU Cai-xia;GAO Gong-min(Comprehensive Technical Service Center of Quanzhou Entry-Exit Inspection and Quarantine Bureau,Fujian Quanzhou 362000, China)

机构地区：[1]泉州出入境检验检疫局综合技术服务中心

出　　处：《广州化工》2019年第17期122-124,148,共4页GuangZhou Chemical Industry

基　　金：国家质量监督检验检疫总局科技计划项目(No:2015IK032);泉州市科技局项目(No:2014Z87)

摘　　要：建立了液相色谱-串联质谱法测定豆芽中金霉素、土霉素、四环素和强力霉素4种四环素类抗生素残留量的方法。样品用0. 1 mol/L EDTA-Mellvaine缓冲液超声提取,HLB柱净化,C18色谱柱分离,正模式下检测。4种四环素类抗生素在5~200μg/L范围内线性关系良好;方法定量限(S/N=10)为1. 5~6. 0μg/kg;添加水平为5、10、20μg/kg时,平均回收率在70. 2%~93. 3%之间;相对标准偏差(RSD,n=6)为8. 5%~13. 7%。方法简单快速,灵敏度高,成功应用于市场上绿豆芽和黄豆芽的检测。A HPLC-MS/MS method was developed for the determination of 4 kinds of tetracycline antibiotics such as chlotetracycline,oxytetracycline,tetracycline and doxycycline residue in bean sprouts. The samples were extracted with0. 1 mol/L EDTA-Mellvaine solution,and cleaned up with HLB column. The chromatographic analysis was carried out on a C18 column with acetonitrile and 0. 1% formic acid solution as the mobile phase in gradient elution program. The results showed that 4 kinds of tetracycline antibiotics showed good linear relationship in the range of 5 ~ 200 μg/L. The limits of quantitation( S/N = 10) was 1. 5 ~ 6. 0 μg/kg. At three spiked concentration levels of 5,10 and 20 μg/kg,the average recovery was 70. 2%~ 93. 3% and relative standard deviation( RSD,n = 6) was 8. 5%~ 13. 7%. The method is simple,rapid and highly sensitive. It has been successfully applied to the detection of mung bean sprout and yellow bean sprouts from the market.

关 键 词：豆芽 液相色谱-串联质谱 四环素类抗生素 

分 类 号：TQ[化学工程]