固相萃取-超高效液相色谱-串联质谱法测定美国进口水果中15种高风险农药及助剂残留

建立了固相萃取-超高效液相色谱-串联质谱 (SPE-UPLC-MS/MS) 测定美国进口水果中15种高风险农药及助剂（乙酰甲胺磷、灭多威、噻虫嗪、噻菌、啶虫脒、西玛津、嘧霉胺、咯菌腈、啶酰菌胺、甲氧虫酰肼、腈菌唑、环酰菌胺、四氟醚唑、增效醚、毒死蜱）残留量的分析方法。样品经破壁机匀浆，乙腈涡旋提取，氨基固相萃取柱净化，岛津Shim-pack XR-ODS色谱柱分离 (75 mm × 2.0 mm，1.6 μm)。采用电喷雾离子源多反应监测模式进行质谱检测，外标法定量。在0.001~0.5 mg/L范围内，15种农药及助剂的质量浓度与对应的峰面积间线性关系良好，R2 ≥ 0.999 5。以梨、葡萄和苹果3种基质为例验证了方法的准确度和精密度。结果表明:在0.005~0.5 mg/kg添加水平下，15种农药及助剂的平均回收率在80%~115%之间，相对标准偏差在5.5%~16%之间，定量限为0.005~0.01 mg/kg。该方法简便、快速、可靠，适用于同时测定水果中上述15种农药及助剂残留。

Determination of 15 high-risk pesticide and adjuvant residues in fruits from USA by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

A method was developed for the quantative determination of 15 high-risk pesticide and adjuvant (acephate, methomyl, thiamethoxam, thiabendazole, acetamiprid,simazine, pyrimethanil, fludioxonil, boscalid, methoxyfenozide, myclobutanil, fenhexamid, tetraconazole, piperonyl butoxide, chlorpyrifos) residues by SPE-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The samples were homogenized, extracted with acetonitrile, and cleaned-up by amino solid phase extraction column. The separation was performed on a Shimadu Shim-pack XR-ODS column (75 mm × 2.0 mm, 1.6 μm). The compounds were identified by MS/MS and multiple reaction monitoring (MRM) mode, and quantified by external standard method. The linearities of 15 pesticides and adjuvants were in the concentration range of 0.001-0.5 mg/L, with the correlation coeffecients higher than 0.999 5. At the fortified levels from 0.005 mg/kg to 0.5 mg/kg in pear, grape and apple, the average recoveries of all 15 pesticides and adjuvants ranged from 80% to 115% with the relative standard deviations varied from 5.5% to 16%. The limits of quantification (LOQs) of the analytes were ranged from 0.005 to 0.01 mg/kg. This method is simple, rapid, accutate and therefore, suitable for the confirmation and quantification of the 15 pesticides and adjuvants in fruits.