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建立了多类粮食作物中15种磺酰脲类除草剂的超高效液相色谱-串联质谱联用仪(UPLC/MS/MS)多离子监测(MRM)的多残留检测方法。样品经乙腈提取,乙腈饱和的正己烷液-液分配,石墨化碳氨基小柱净化,采用UPLC-MS/MS(ESI+)测定。方法中各种磺酰脲类除草剂在5～200μg/L浓度范围内线性良好,相关系数在0.9995～0.9999。在5～100μg/kg范围内,平均加标回收率在71.6%～115.3%之间,相对标准偏差不大于15%。各种药物的定量限(S/N≥10)均可达到5μg/kg。该方法可同时满足大豆、大米、玉米等多种粮食中磺酰脲类除草剂的检测需求。
A multi-residue detection method based on UPLC / MS / MS multi-ion monitoring (MRM) was developed for 15 sulfonylurea herbicides in many kinds of food crops. The sample was extracted with acetonitrile, saturated with acetonitrile, liquid-liquid, and purified by carbonitride cartridges. The samples were determined by UPLC-MS / MS (ESI +). The method of various sulfonylurea herbicides in the range of 5 ~ 200μg / L linear within good range, the correlation coefficient of 0.9995 ~ 0.9999. In the range of 5 ~ 100μg / kg, the average recoveries ranged from 71.6% to 115.3%, and the relative standard deviations were no more than 15%. The limits of quantification of various drugs (S / N≥10) can reach 5μg / kg. The method can simultaneously meet the detection requirements of sulfonylurea herbicides in a variety of foods such as soybean, rice and corn.