利用基质分散固相萃取技术（dSPE）结合GC-MS/MS分析，建立了皂角米中73种不同极性农药残留的快速筛查方法。皂角米样品用酸化乙腈经振荡提取和超声辅助提取，然后加入萃取包高速离心，取上清液加入纯化管中再进行分散固相萃取净化，采用多反应监测扫描模式（MRM）进行监测，基质匹配溶液内标法定量。各目标物在不同范围内呈良好的线性相关，相关系数（R2）均不小于0.990，方法的定量限（LOQ，S/N=10）为2.5~20.0 μg/kg。在皂角米基质中进行加标回收考察试验，平均回收率为68.6%~110.7%，相对标准偏差RSD（n=6）在2.1%~9.7%之间。与传统前处理方法QuEChERS法相比，分散固相萃取技术在检测成本和处理速度上有一定优势，且一次进样可同时分析73种农药，准确、灵敏。该方法可为日后在食品风险监测领域对粮食中农药残留的筛查和确证、风险评估、定量仲裁等研究提供了技术支持。

A rapid screening method for 73 pesticide residues of different polarities in Gleditsia sinensis was established by matrix solid-phase dispersion extraction (dSPE) combined with GC-MS/MS analysis. The Gleditsia sinensis seed samples were extracted with acidified acetonitrile by shaking and ultrasonic-assisted extraction, and then added to the extraction bag for high-speed centrifugation. The supernatant was added to the purification tube and then subjected to dispersive solid-phase extraction purification. Multi-reaction monitoring scanning mode (MRM) was used for monitoring, and the matrix matching solution internal standard method was used for quantification. Each target had a good linear correlation in different ranges, with the correlation coefficients (R2) not lower than 0.990, and limits of quantification (LOQs) in the range of 2.5 ~ 20. 0 μg/kg (S/N=10). In the spiked Gleditsia sinensis seed matrix, the average recovery rates were 68.6%~110.7% with the relative standard deviations (RSDs, n=6) between 2.1% and 9.7%. Compared with the traditional pretreatment method, QuEChERS, the dispersive solid-phase extraction technology has certain advantages in detection cost and processing speed, and can analyze 73 pesticides simultaneously by one injection with high accuracy and sensitivity. This method can provide technical support for future research on the screening and confirmation of pesticide residues in food, risk assessment, and quantitative arbitration in the field of food risk monitoring.

国家重点研发计划项目（2017YFC1601806；2017YFC1601805）；黔科合支撑[2017]2972