UPLC-MS/MS法检测稻米及土壤中扑草净除草剂的残留量

Determination of Prometryn Residues in Rice and Soil by UPLC-MS/MS

建立检测稻米及土壤中扑草净的UPLC-MS/MS方法.稻米和土壤样品经乙腈和混合液提取,甲醇/二氯甲烷溶解,PSA固相萃取柱净化,氮气吹干后经UPLC-MS/MS测定,外标法定量.建立了水稻及土壤中提取扑草净残留量的液相色谱-质谱/质谱测定方法.扑草净在稻米及土壤中的最低检测质量分数分别为0.01 mg/kg;最小检出量5×10～11g;稻米添加回收率为82.7％～105.3％,土壤中添加回收率为79.6％～103.3％;稻米的RSD为2.6％～3.6％,土壤的RSD为3.2％～5.2％.建立方法准确、快速、灵敏度高,能够满足扑草净残留量分析的要求.

Established the method for the determination ofprometryn residuesin rice and soil by UPLC-MS/MS. Rice and soil samples were extracted with the solution of aeetonitrile andwater and dissolvedin methanol/dichloromethane. After purified by PSA solid-phase extraction （SPE） and nitrogen drying, the samples were measured by UPLC-MS/MS usingexternal standardquan- tification. The method for the determination of prometryn residues in rice and soil by UPLC-MS/ MS was established. The limit of quantification was 0.01mg/kg both in rice and soil with the limit of detectable amount of 5×l0~llg; the recoveries were 82.7%~105.3%in rice and 79.6%- 103.3% in soil; the RSD was 2.6%-3.6% in rice and 3.2%-5.2% in soil. The method is accu- rate, rapid and sensitiveenough to be used forprometryn residueanalysis.