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高效液相-串联质谱法测定餐饮冷菜中的庆大霉素残留量 被引量:4

Gentamicin residue in cold dishes determined by high performance liquid chromatography-tandem mass spectrometry
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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20μg/kg;在20~500μg/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。 [Objective]To establish a method for the determination of gentamicin residue in cold dishes by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).[Methods]Maigre 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.[Results]The detection limit of gentamicin residue was 20μg/kg.The method showed a good linearity over the range of 20-500μg/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).[Conclusion]The established method is highly sensitive and accurate,which is suitable for the detection of gentamicin residue in cold dishes.
作者 刘晓云 迟秋池 夏苏捷 陈燕 王柯 LIU Xiao-yun;CHI Qiu-chi;XIA Su-jie;CHEN Yan;WANG Ke(Shanghai Institute of Food and Drug Control,Shanghai 201203,China)
出处 《上海预防医学》 CAS 2018年第6期468-471,共4页 Shanghai Journal of Preventive Medicine
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 gentamicin high performance liquid chromatography-tandem mass spectrometry solid phase extraction cold dishes
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