固相萃取-超高效液相色谱-质谱/质谱法同时测定蔬菜中7种杀菌剂的残留量

SPE UPLC-MS/MS determination of residual of 7 kinds of microbicides in vegetables

建立了采用固相萃取-超高效液相色谱-质谱/质谱法(SPE-UPLC-MS/MS)对蔬菜中7种杀菌剂农药(霜脲氰、嘧霉胺、甲霜灵、咪鲜胺、戊唑醇、丙环唑、苯醚甲环唑)残留同时测定的方法。样品用乙腈提取后经石墨化碳氨基复合固相萃取柱净化处理,经Acquity UPLCTM BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离后测定,该方法采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好(r2>0.994)。检出限为0.0006～0.002 mg/kg,总体回收率为87.5%～98.6%,相对标准偏差为3.4%～9.0%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为蔬菜中相关药物残留的筛选检测方法。

Residual amounts of 7 kinds of microbicides（cymoxanil,pyrimethanil,metalaxyl,prochloraz,tebuconazole,propiconazole and difenoconazole） were determined by SPE-UPLC-MS/MS.The sample was extracted with acetonitrile and extrac was purified on Carb/NH2 SPE column.The eluate was separated by gradient elution with methanol,formic acid and water solution of different ratio on Acquity UPLCTM BEH C18（100 mm×2.1 mm,1.7 μm） column and determined by LC-MS/MS,using positive-ion electrospray ionization in multiple reaction monitoring（MRM） mode.External standard method was used to determine the residue contents with a good linear relationship（r20.992）.The limits of quantification（LOQ） was 0.0006～0.002 mg/kg.The recovery ranges were from 87.5% to 98.6% with the relative standard deviations（RSDs） between 3.4% and 9.0%.As a screening method,the developed procedure is suitable for the determination and confirmation of the bdrug residues in vegetables samples.