UPLC-MS/MS检测小麦中甲哌鎓的残留量

Determination of Mepiquat Chloride Residue in Wheat by UPLC-MS/MS

本研究建立了采用超高效液相色谱-串联质谱(UPLC-MS/MS),测定小麦籽粒和秸秆中甲哌鎓残留量的分析方法。样品采用乙酸铵-0.1%甲酸水溶液和甲醇提取,提取液经分散固相萃取净化,采用多反应监测模式(MRM),外标法定量测定。结果表明:在0.05~5 mg/L范围内,甲哌鎓的质量浓度与其峰面积呈良好的线性关系(相关系数大于0.999)。添加水平为0.05、0.5、1 mg/kg时,检测方法的平均回收率为78%~103%,相对标准偏差为2.3%~8.9%。此分析方法的线性关系良好,灵敏度和精确性满足农药残留分析要求,可用于生产上小麦中甲哌鎓残留检测分析。

Ultra performance liquid chromatography tandem-mass spectrometry(UPLC-MS/MS)method was established for the determination of mepiquat chloride residue in wheat grain and stalk.The samples were extracted by ammonium acetate-formic acid aqueous solution and methanol,purified by dispersed solid phase extraction,quantified by external standard method using multiple reaction monitoring mode(MRM).The results showed that there were good linear relationships between the peak areas of mepiquat chloride and their mass concentrations in the range of 0.05-5 mg/L.The recoveries were 78%to 103%with relative standard deviations of 2.3%-8.9%at the fortified levels of 0.05,0.5 and 1 mg/kg.The method was sensitive and acurate with good linear relationship,which accorded with the requirements of pesticide residue analysis,could be used for analysing mepiquat chloride residue.