QuEChERS法和UPLC-MS-MS法快速测定稻谷中4种磺酰脲类除草剂的残留量

Using Qu ECh ERS method to rapidly determine four sulfonylurea herbicides in unhusked rice samples by ultra performance liquid chromatography-mass spectrometry

建立了Qu ECh ERS法-超高效液相色谱串联质谱法（UPLC-MS-MS）快速测定稻谷中氯磺隆、甲磺隆、苄嘧磺隆、醚磺隆4种磺酰脲类除草剂的方法。采用酸化乙腈超声提取,Qu ECh ERS法净化的方法处理稻谷样品,利用UPLC-MS-MS分析,在多反应监测（MRM）模式下以0.1%甲酸水和乙腈为流动相等度洗脱。4种除草剂在10~200μg/L范围内线性良好,相关系数在0.995~0.998之间,平均加标回收率为75.2%~113.3%,相对标准偏差在0.6%~8.3%之间。该方法适用于稻谷中4种除草剂残留的测定。

A method was developed for the simultaneous determination of four sulfonylurea herbicides in unhusked rice by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry, Unhusked rice samples were extracted with acidified acetonitrile by ultrasonic wave and purified by QuEChERS method. The purified liquid was analysed by UPLC-MS-MS in multiple reaction monitoring （MRM） mode. 0.1% formic acid in water and acetonitrile were used as mobile phase to complete isocratic elution. The linear ranges of 4 herbicides were 10-200 IJg/L and the correlation coefficients were 0.995-0.998. The average recoveries were in the range of 75.2%-113.3%. The relative standard deviations were between 0,6% and 8.3%. The method can be used for determination of herbicides in unhusked rice.