在线凝胶渗透色谱-气相色谱串联质谱法测定动物源性食品中氯霉素  

Determination of chloramphenicol in animal derived food by on-line gel permeation chromatography-gas chromatography-tandem mass spectrometry

作　　者：劳哲[1] 江恩源[1] 朱国强[1] LAO Zhe;JIANG Enyuan;ZHU Guoqiang(Physical and ChemicalInspection Section of Wuzhou Center for Disease Control and Prevention,Wuzhou 543002)

机构地区：[1]梧州市疾病预防控制中心理化检验科,梧州543002

出　　处：《分析试验室》2020年第6期726-730,共5页Chinese Journal of Analysis Laboratory

基　　金：梧州市科学研究与技术开发计划项目(201702131)资助。

摘　　要：建立了在线凝胶渗透色谱-气相色谱串联质谱(GPC-GC-MS/MS)测定动物源性食品中氯霉素的方法。样品经提取、净化、衍生化和定容后,用大体积进样装置取100μL进样,过凝胶渗透色谱柱后由切换阀排出残留的脂肪和色素等大分子物质,剩余的组分经色谱柱分离,质谱选择EI源多反应监测模式(MRM)检测,内标法定量。氯霉素浓度在0. 25~10 ng/mL范围内和其衍生物与内标衍生物的峰面积比呈线性关系,相关系数r=0. 9976,检出限为0. 05μg/kg,在低、中和高3个添加水平下,回收率在84. 0%~96. 1%之间;RSDs在2. 1%~8. 2%之间。该方法检出限低,精密度和准确度高,适用于动物源性食品中氯霉素的测定。A method was developed for the determination of chloramphenicol(CAP)in animal-derived food by on-line gel permeation chromatography-gas chromatography-tandem mass spectrometry(GPC-GC-MS/MS).After extraction,purification,derivatization and constant volume,a 100μL of the product was injected into GPC-GC-MS/MS by large-volumesampling device.Once it purified through gel-penetration chromatographic column,the residues of fat,pigmen,and other macromolecular substances were excluded via the switchingvalves.The residual product was then separated through chromatographic column.The EI multi-reaction monitor mode(MRM)was chosen for the mass spectrum,and the internal standard methodology was employed.Whenthe target CAP concentration was in the range of 0.25-10 ng/mL,it showed a good linear relationship with the peak area ratio of the derivatives and the internal standard derivatives,the correlation coefficient(r)was 0.9976 with the LOD of 0.05μg/kg.Under the low,medium and high spiked levels,the recoveries were in the range of 84.0%-96.1%,and theRSDs were in the range of 2.1%-8.2%.The method has a lower detection limit,as well as a higher precision and accuracy,indicating a application prospect of CAP determination in animalderived food.

关 键 词：在线凝胶渗透色谱 气相色谱串联质谱 大体积进样装置 动物源性食品 氯霉素 

分 类 号：O657.63[理学—分析化学]