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氨基糖苷类药物的危害及其检测方法研究进展
引用本文:刘晓云, 迟秋池, 夏苏捷, 陈燕, 王柯. 高效液相-串联质谱法测定餐饮冷菜中的庆大霉素残留量[J]. 上海预防医学, 2018, 30(6): 468-471. DOI: 10.19428/j.cnki.sjpm.2018.18813
作者姓名:刘晓云  迟秋池  夏苏捷  陈燕  王柯
作者单位:上海市食品药品检验所, 上海 201203
摘    要:目的建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定餐饮冷菜中的庆大霉素残留量的方法。方法素鲍鱼样品经磷酸盐缓冲液提取,C18固相萃取柱净化、浓缩后,使用七氟丁酸作为离子对试剂,Inertsil ODS-3色谱柱进行分离,HPLC-MS/MS法进行测定,以外标法定量。结果庆大霉素的检出限为20 μg/kg;在20~500 μg/kg范围内线性关系良好, 相关系数r>0.99;平均回收率在90.49%~102.9%之间,相对标准偏差为4%~9%(n=6)。结论本方法灵敏、快速,可用于餐饮冷菜中庆大霉素残留量的检测。

关 键 词:庆大霉素  高效液相色谱-串联质谱法  固相萃取  餐饮冷菜
收稿时间:2018-04-15

Development of an improved high resolution mass spectrometry based multi-residue method for veterinary drugs in various food matrices
Xiao-yun LIU, Qiu-chi CHI, Su-jie XIA, Yan CHEN, Ke WANG. Gentamicin residue in cold dishes determined by high performance liquid chromatography-tandem mass spectrometry[J]. Shanghai Journal of Preventive Medicine, 2018, 30(6): 468-471. DOI: 10.19428/j.cnki.sjpm.2018.18813
Authors:Xiao-yun LIU  Qiu-chi CHI  Su-jie XIA  Yan CHEN  Ke WANG
Affiliation:Shanghai Institute of Food and Drug Control, Shanghai 201203, China
Abstract:ObjectiveTo establish a method for the determination of gentamicin residue in cold dishes by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).MethodsMaigre abalone was extracted with phosphate buffer, then the extracts were purified by a C18 catridge.The gentamicin residue was separated by Inertsil ODS-3 column, heptafluorobutyric acid as the ion-pair reagent, and detected by HPLC-MS/MS with external standard method for quantification.ResultsThe detection limit of gentamicin residue was 20 μg/kg.The method showed a good linearity over the range of 20-500 μg/kg with r > 0.99.The average recoveries were in the range of 90.49%-102.9%, while the relative standard deviations (RSD) were 4%-9% (n=6).ConclusionThe established method is highly sensitive and accurate, which is suitable for the detection of gentamicin residue in cold dishes.
Keywords:gentamicin  high performance liquid chromatography-tandem mass spectrometry  solid phase extraction  cold dishes
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