高效液相色谱-串联质谱法测定稻米和稻壳中井冈霉素A的残留

Determination of Validamycin A Residues in Rice and Rice Hull by High Performance Liquid Chromatography-Tandem Mass Spectrometry

本文建立了稻米和稻壳中井冈霉素A的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品用甲醇-水(9+1)涡旋提取,过滤膜后进行HPLC-MS/MS分析。用多反应监测技术确定井冈霉素A的两对离子对m/z498.2/178.1、m/z498.2/336.1为定性离子对,m/z498.2/178.1为定量离子对。方法的线性范围为0.005～0.2mg/L,其中稻壳的线性相关系数为0.9993,稻米的线性相关系数为0.9988。稻米、稻壳的0.05、0.1、0.5 mg/kg三个浓度的添加回收率为71.6%～88.8%,相对标准偏差(RSD)为1.89%～8.16%。方法的定量限(LOQ)为5μg/kg。

A method for the determination of validamycin A residues in rice and rice hull was developed using high performance liquid chromatography-tandedm mass spectrometry（HPLC-MS/MS）.Validamycin A was vortex extracted with methanol-water（9＋1,V/V） and then analyzed by HPLC-MS/MS.For the samples,the recoveries ranged from 71.6% to 88.8% and the relative standard deviations（RSDs） ranged from 1.9% to 8.2% were obtained.The limit of quantification（LOQ） was 5 μg/kg with a linear range of 0.005 to 0.2 mg/L.