免疫亲和注射器微萃取-高效液相色谱串联质谱法测定牛奶中玉米赤霉醇类化合物  

Determination of Zeranols in Milk Using Immunoaffinity Microextraction in a Packed Syringe and High Performance Liquid Chromatograph-Tandem Mass Spectrometry

作　　者：张欣达 李娜 赵世瑾 郑妍 杨琳燕 张伟 李留安 李存 ZHANG Xinda;LI Na;ZHAO Shijin;ZHENG Yan;YANG Linyan;ZHANG Wei;LI Liu′an;LI Cun(College of Animal Science and Veterinary Medicine/Tianjin Key Laboratory of Agricultural Animal Breeding and Healthy Husbandry,Tianjin Agricultural University,Tianjin 300384,China;Tianjin Beidagang Wetland Management Center,Tianjin 300270,China;Tianjin Institute of Quality Standards and Testing Technology for Agricultural Products,Tianjin 300381,China)

机构地区：[1]天津农学院动物科学与动物医学学院/天津市农业动物繁育与健康养殖重点实验室,天津300384 [2]天津市北大港湿地自然保护区管理中心,天津300270 [3]天津市农业质量标准与检测技术研究所,天津300381

出　　处：《食品与生物技术学报》2023年第5期29-34,共6页Journal of Food Science and Biotechnology

基　　金：国家自然科学基金项目(31372482);天津市“131”创新型人才团队项目(JRC2018044);天津市奶牛(肉羊)产业技术体系创新团队建设项目(ITTCRS2021000)。

摘　　要：将偶联玉米赤霉醇单克隆抗体的二氧化硅作为注射器微萃取的选择性吸附剂,建立了检测牛奶中6种玉米赤霉醇类化合物(ZERs)的免疫亲和注射器微萃取-高效液相色谱串联质谱法(IA-MEPS-LC-MS/MS)。将牛奶离心后,取中间夹层,使用免疫亲和注射器微萃取,超纯水洗涤,甲醇洗脱,洗脱液浓缩,流动相复溶后进行LC-MS/MS分析,采用C18色谱柱分离,水-乙腈为流动相梯度洗脱。使用基质匹配外标法定量,在工作液质量浓度0.1~100.0 ng/mL时6种ZERs线性良好,相关系数在0.9943~0.9962;在ZERs添加水平为1 ng/g时,平均回收率在50.40%~68.34%,日内RSD在4.87%~17.64%,日间RSD在7.04%~18.75%,本方法的检测限(LOD)为0.05 ng/g,定量限(LOQ)为0.2 ng/g。This research prepared a selective adsorbent on the basis of SiO2 glass beads bound with zeranol monoclonal antibody and the method of immunoaffinity microextraction in a packed syringe and high performance liquid chromatograph-tandem mass spectrometry(IA-MEPS-LC-MS/MS)was further developed to detect six kinds of zeranols(ZERs)in milk.Milk samples were centrifuged,and the middle layer was extracted with IA-MEPS syringe and washed by ultra-pure water before eluted with methanol.The eluent was concentrated and then re-dissolved by mobile phase.Finally,the sample was detected by LC-MS/MS,separated on a C18 column with the mobile phase of water and acetonitrile.Matrix-matched external standard method was used for quantification.The linearity of six ZERs was good within 0.1~100.0 ng/mL,and the correlation coefficient was 0.9943~0.9962.The average recoveries ranged from 50.40%to 68.34%at the addition level of 1 ng/g,the intra-day and the inter-day RSDs were 4.87%~17.64%and 7.04%~18.75%,respectively.The limit of detection(LOD)and limit of quantification(LOQ)of this method were 0.05 ng/g and 0.2 ng/g,respectively.

关 键 词：玉米赤霉醇类化合物 免疫亲和注射器微萃取 牛奶 残留检测 

分 类 号：O657.63[理学—分析化学] TS251.51[理学—化学]