在系统优化固相萃取吸附剂填料类型、洗脱溶剂种类及体积的基础上，建立了牛奶和奶粉中213种农药残留的气相色谱-三重四极杆串联质谱（ GC-MS／MS）方法。试样用乙腈均质提取，采用石墨化炭黑／氨基柱（ ENVI-Carb／NH2）净化后，用 GC-MS／MS多反应离子监测（MRM）模式进行检测，外标法定量。结果表明，197种农药在10~1000μg／L，16种农药在50~1000μg／L范围内线性关系良好，相关系数均大于0.99，方法的检出限（ S／N=3）为0.03~7.59μg／kg，定量限（ S／N=10）为0.10~21.94μg／kg，平均添加回收率为66.9％~120.1％，相对标准偏差（ RSD）为1.23％~17.6％。该方法样品处理简单快速，相比其他多残留分析方法净化效果好，灵敏度和选择性高，适用于日常检测工作。
On the basis of the optimization of solid phase extraction adsorbent,eluting solvent types and amounts,a gas chromatography-triple quadrupole tandem mass spectrometry( GC-MS/MS)method was established for the determination of 213 pesticide residues in milk and milk power. The samples were extracted by acetonitrile,cleaned-up with an ENVI-Carb/NH2 solid-phase extractant,and determined by GC-MS/MS using external standard method. The linear ranges were from 10 to 1 000 μg/L for 197 pesticides,from 50 to 1 000 μg/L for the other 16 pesticides with the correlation coefficients higher than 0. 99. The limits of detection( LODs, S/N=3)varied over the range of 0. 03 to 7. 59 μg/kg,and limits of quantification( LOQs,S/N=10)ranged from 0. 10 to 21. 94 μg/kg. The average recoveries in different matrices were in the range of 66. 9%-120. 1% with the relative standard deviations( RSDs ) of 1. 23%-17. 6%. This method is simple,rapid,sensitive and reliable for meeting the requirements for the simul-taneous identification and quantification of the multi-residues in milk and milk power.
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