QuEChERS法和UPLC-MS-MS法快速测定棉籽中的马拉硫磷

目的]建立超高效液相色谱-串联质谱(UPLC-MS-MS)对棉籽中马拉硫磷的检测方法。方法]棉籽样品经乙腈提取,正交试验优化QuEChERS净化方法,正离子多反应监测(MRM)模式测定。结果]该方法在0.01~1.00 mg/L线性关系良好,相关系数为0.999 9,最低检出量为2μg/kg,最低检出浓度为10μg/kg,加标回收率82.29%~90.64%,相对标准偏差在5.25%~14.64%。结论]该方法简便、快速、准确、灵敏,节省有机溶剂,环境友好,适合大批量棉籽中马拉硫磷的检测需要。

Using QuEChERS and UPLC-MS-MS Method to Rapidly Determine Malathionin in Cotton-seed

Objective] A method was developed for determination of malathion in cotton-seed by using ultra performance liquid chromatography-tandem mass spectrometry.Method] The samples were extracted by acetonitrile, the QuEChERS purification method was optimized by orthogonal array design and the positive ion multiple reaction monitoring (MRM) mode was used.Result] The results showed that the linear ranges of malathion were 0.01-1.00 mg/L and the correlation coefficient was 0.999 9.The minimum detectable quantity and minimum detectable concentration were 2 μg/kg and 10 μg/kg respectively.The average recoveries were in the range of 82.29%-90.64%.The relative standard deviations were between 5.25% and 14.64%.Conclusion] The method is proved to be simple, fast, accurate, sensitive, saving organic solvents, suitable for mass detection of actual needs.