QuEChERS-超高效液相色谱串联质谱法测定水产品中红霉素残留  

QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry for the determination of erythromycin in fishy products

作　　者：严忠雍[1,2] 张小军[1,2] 李佩佩[1,2] 方益[1,2] 喻亮[1,2] 张帅[1,2] 祝银[1,2] 李强[3] 

机构地区：[1]浙江省海洋水产研究所,浙江舟山316021 [2]浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316021 [3]中国水产科学研究院,北京100141

出　　处：《浙江大学学报（理学版）》2017年第3期339-344,共6页Journal of Zhejiang University（Science Edition）

基　　金：公益性行业(农业)科研专项(201503108);浙江省公益性技术研究项目(2014C32087)

摘　　要：建立了超高效液相色谱串联质谱法测定水产品中的红霉素残留量.样品用改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)进行提取净化,经乙腈快速提取,无水硫酸镁和氯化钠除水后,用N-丙基乙二胺(PSA)净化,液相色谱串联质谱分析测定.在ACQUITY UPLC BEH C_(18)色谱柱上进行分离,采用梯度洗脱,以0.1%甲酸水溶液和甲醇为流动相,电喷雾正离子电离,多反应监测模式,内标法定量.结果表明:红霉素浓度在0.5~50μg·L^(-1)时具有良好的线性关系,相关系数为0.997 6,定量限为0.3μg·kg^(-1),回收率为87.6%~96.1%,相对标准偏差为2.2%~5.3%.本方法操作简易、应用性强,适合水产品中红霉素的常规检测.A method has been developed for the determination of erythromycin in fishery products by ultra performance liquid chromatography-tandem mass spectrometry.The samples were pretreated using the modified QuEChERS（Quick,Easy,Cheap,Effective,Rugged,Safe）method that completed the extraction and clean-up steps in one procedure.The samples were extracted with acetonitrile,dehydrated with sodium chloride and anhydrous magnesium sulfate,and cleaned up by dispersive solid phase extraction on primary secondary amine,and then were detected by HPLC-MS/MS.The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution using methanol and 0.1%formic acid solution as mobile phase.Internal standard method was used for quantification,and the positive electrospray ionization source was applied under the multiple reaction monitoring mode.Linear ranges of erythromycin was in the range of 0.5to 50.0μg·L-1 with correlation coefficient of 0.997 6.The quantification limit of the method was 0.3μg·kg-1.The recoveries of erythromycin were from 87.6%to 96.1%,and the relative standard deviation was from 2.2%to 5.3%.The method was simple,fast and sensitive for the analysis of erythromycin in fishy products.

关 键 词：QUECHERS 液相色谱串联质谱 水产品 红霉素 

分 类 号：O657.6[理学—分析化学] P76[理学—化学]