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本文确定了牛乳中检测的52种农药残留污染物。利用气相色谱串联质谱(GC-MS/MS),建立了52种农药残留污染物在牛乳中的分析方法。本文方法改进在于:通过农药残留的传播途径和在牛体内的代谢方式,确定了牛乳中可能存在的52种农药残留污染物,大大缩小了牛乳中农药残留污染物的筛查范围;简化了分组测定,实现一次处理样品,一次进样,可完成52种农残组分的同时测定,简化了其它方法分组测定方式,极大地提高了检测效率和检测通量;对气相色谱条件进行了优化(进样口温度对52种不同组分灵敏度的影响),对质谱条件进行了优化(SRM多选择离子的确定,最佳碰撞能量的确定)。比较了不同样品净化方法对回收率的影响(C18固相小柱萃取法和固相分散萃取法),最终确定C18固相小柱萃取法净化样品。本方法结果表明,本方法52种农残在相应的添加水平下,平均加标回收率(n=6)为60.5%~111.5%,测定结果相对标准偏差(RSD)为1.94%~9.67%,方法的检出限(S/N=3)为0.0007~0.013mg/kg。本文为生鲜牛乳的农药残留指标评价提供了一种简便﹑实用的检测方法。采用本方法测定500个不同地域的生鲜牛乳样品,收到了良好的效果。
This article identified 52 pesticide residue contaminants detected in milk. Using GC-MS / MS, 52 pesticide residue contaminants in milk were analyzed. The improvement of the method in this paper is that through the pesticide route of transmission and the metabolism in cattle body, we can determine the remaining pesticide residues in 52 pesticide residues in milk, greatly reduce the screening scope of pesticide residues in milk and simplify the grouping Measurement, to achieve a sample processing, a sample can be completed at the same time 52 kinds of pesticide residues in the determination of the same time, simplifying the determination of other methods grouping method, which greatly improves the detection efficiency and detection flux; gas chromatographic conditions were optimized The effect of inlet temperature on the sensitivity of 52 different components) was optimized for MS conditions (SRM multiple choice ion determination, best collision energy determination). The effects of different sample decontamination methods on the recovery rate were compared (C18 solid phase cartridge extraction and solid phase dispersion extraction), and finally the C18 solid phase cartridge extraction method was used to purify the sample. The results of this method showed that the average recoveries (n = 6) of 60 kinds of pesticide residue of this method were 60.5% ~ 111.5% at the corresponding additive levels, and the relative standard deviations (RSDs) were 1.94% ~ 9.67% The detection limit (S / N = 3) of the method was 0.0007 ~ 0.013mg / kg. This paper provides a simple and practical method for the evaluation of pesticide residues in fresh milk. Using this method to determine 500 different regions of fresh milk samples, received good results.