基于HPLC-MS/MS测定替考拉宁中4种黄曲霉毒素  

Determination of 4 aflatoxins in Teicoplanin by HPLC-MS/MS

作　　者：赵二强 雒金霞 和燕玲 邵伍军 吴春艳 ZHAO Erqiang;LUO Jinxia;HE Yanling;SHAO Wujun;WU Chunyan(Zhejiang Hisun Pharmaceutical Co.,Ltd.,Taizhou Zhejiang 318000,China;Taizhou Vocational College of Science&Technology,Taizhou Zhejiang 318000,China)

机构地区：[1]浙江海正药业股份有限公司,浙江台州318000 [2]台州科技职业学院,浙江台州318000

出　　处：《中兽医医药杂志》2024年第5期79-82,共4页Journal of Traditional Chinese Veterinary Medicine

基　　金：浙江省2023年度高校国内访问工程师校企合作项目(FG2023323)。

摘　　要：建立高效液相色谱-三重四极杆质谱法(HPLC-MS/MS)测定替考拉宁中4种黄曲霉毒素AFB1、AFB2、AFG1、AFG2。样品经溶解、萃取、氮气吹干、再溶解处理,去除了基质对目标物检测的干扰;处理样品经C_(18)色谱柱梯度洗脱分离,采用电喷雾离子源与正离子多反应监测(MRM)模式采集三重四极杆质谱数据,对替考拉宁中4种黄曲霉毒素同时进行检测。4种黄曲霉毒素在4.000 0~80.000 0 ng/L质量浓度范围内具有良好的线性关系,相关系数r>0.999 9;检测限为0.06μg/kg,定量限为0.20μg/kg;回收率为85.3%~95.0%,RSD为3.3%~3.6%。对3批替考拉宁样品中的黄曲霉毒素进行检测,均未检到黄曲霉毒素AFB1、AFB2、AFG1、AFG2。本方法操作简捷,灵敏度高,准确性好,适合于替考拉宁中黄曲霉毒素的定量测定。To establish a HPLC-MS/MS(high-performance liquid chromatography triple quadrupole mass spectrometry)method for the determination of 4 aflatoxins in Teicoplanin.Sample was dissolved,extracted,dried with nitrogen gas,and then dissolved again to remove the interference of the substrate for detection of 4 aflatoxins.The treated samples were separated by gradient elution on a C18 chromatographic column,and the triple quadrupole mass spectrometry was used to collect data using the positive mode,ion electrospray ionization(ESI)source and MRM(multi reaction monitoring)mode.The 4 aflatoxins(AFB1,AFB2,AFG1,and AFG2)were simultaneously detected by HPLC-MS/MS in Teicoplanin.The correlation coefficient(r)of 4 aflatoxins in the concentration range of 4.0000-80.0000 ng/L was greater than 0.9999;the detection limit was 0.06µg/kg,and the quantification limit was 0.20µg/kg;the recovery rate was between 85.3%and 95.0%,and the RSD was between 1.3%and 3.6%.Aflatoxin AFB1,AFB2,AFG1,and AFG2 were not detected in the three batches of samples of Teicoplanin.This method is simple to operate,highly sensitive,and accurate,which is suitable for the quantitative determination of aflatoxin in Teicoplanin.

关 键 词：高效液相色谱 三重四极杆质谱 替考拉宁 黄曲霉毒素 

分 类 号：S859.1[农业科学—临床兽医学]