高效液相-串联质谱法测定餐饮冷菜中的庆大霉素残留量

刘晓云; 迟秋池; 夏苏捷; 陈燕; 王柯

doi:10.19428/j.cnki.sjpm.2018.18813

高效液相-串联质谱法测定餐饮冷菜中的庆大霉素残留量

Gentamicin residue in cold dishes determined by high performance liquid chromatography-tandem mass spectrometry

摘要

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。

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.

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