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    超高效液相色谱-串联质谱法测定蜂蜜中的14种杀虫剂残留

    Determination of Residues of 14 Insecticides in Honey by UPLC-MS/MS

    • 摘要: 采用超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定蜂蜜中的14种杀虫剂残留,并对自制的毒死蜱-D10同位素内标的适用性进行筛选。样品经乙腈提取,氨基净化柱净化后,以ACQUITY UPLC BEH C18色谱柱为分析柱,甲醇-2 mmol·L-1甲酸铵溶液混合液为流动相进行梯度洗脱,质谱中选择电喷雾正离子源和多反应监测模式。经验证毒死蜱、噻螨酮、炔螨特、蝇毒磷、倍硫磷、伏杀硫磷、甲基嘧啶磷、甲基毒死蜱可用毒死蜱-D10作为内标进行定量,吡螨胺、哒螨灵、螺螨酯、乙螨唑、唑螨酯、杀螟硫磷则用基质匹配法定量。14种杀虫剂的线性范围为1.0~200 μg·L-1,检出限(3S/N)为0.01~0.20 μg·kg-1,测定下限(10S/N)为0.03~0.50 μg·kg-1。加标回收率在81.9%~129%之间,测定值的相对标准偏差(n=6)不大于11%。

       

      Abstract: UPLC-MS/MS was applied to the simultaneous determination of residues of 14 insecticides in honey, with the applicability screening for homemade chlorpyrifos-D10 as the isotope internal standard. The sample was extracted with acetonitrile, and the extract was cleaned up with amino purification column. The purified solution was separated on an ACQUITY UPLC BEH C18 chromatographic column with a mixture of methanol and ammonium formate solution (2 mmol·L-1) as the mobile phase for gradient elution. Electrospray ionization in positive mode and the multi-reaction monitoring mode were adopted in MS analysis. Chlorpyrifos, propargite, hexythiazox, coumaphos, fenthion, phosalone, chlorpyrifos-methyl and pirimiphos-methyl were proved to be suitable for internal standard quantification; while tebufenpyrad, pyridaben, spirodiclofen, etoxazole, fenpyroximate and fenitrothion were quantitified with matrix matching method. The same linearity range of 14 insecticides was 1.0-200 μg·L-1, with detection limits (3S/N) of 0.01-0.20 μg·kg-1 and the lower limits of determination (10S/N) of 0.03-0.50 μg·kg-1. Recovery rates obtained by standard additon mehtod ranged from 81.9% to 129% and RSDs (n=6) were within 11%.

       

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