气相色谱/三重四极杆串联质谱法测定牛奶及奶粉中213种农药多残留

Determination of 213 pesticide residues in milk and milk power by gas chromatography-triple quadrupole tandem mass spectrometry

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（ENVICarb/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10~1 000μg/L,16种农药在50~1 000μg/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（GCMS / 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 / NH2solid-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 other16 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 simultaneous identification and quantification of the multi-residues in milk and milk power.