摘要
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。
In this paper, 52 kinds of pesticide residues in milk were determined. Based on gas chromatography tandem mass spectrometry （GC-MS/MS）., 52 methods for the analysis of pesticide residues in milk were established. This improved method is： through the transmission of pesticide residues and metabolism in vivo in cattle, the pollutants may exist 52 kinds of pesticide residues in milk, greatly narrowing the scope of screening of pesticide residue in milk contamination; Simplifies the packet determination, a sample, a sample of 52 kinds of pesticide residues, can be completed at the same time the determination of components, greatly improves the detection efficiency and the detection flux; The conditions of gas chromatography were optimized （the effect of inlet temperature on the sensitivity of the 52 different components）, and the conditions of mass spectrometry were optimized. The determination of the best collision energy was determined by SRM. comparison of different sample purification methods to influence the recovery rate （C18 solid-phase extraction and, solid-phase extraction method）, and ultimately detemfine the C18 solid-phase extraction and purification of samples .This method is a sample, a sample of 52 kinds of pesticide residues, can be completed at the same time the determination of components, simplifies the other grouping method determination method, greatly improves the detection efficiency and the detection flux. The results show that the method of 53 kinds of pesticide residues in the corresponding addition level, the average recoveries （n=6） ranged from 60.5% to 111.5%, the relative standard deviation of the determination results （RSD） ranged from 1.94% to 9.67%, the detection limit （S/N=3） ranged from 0.0007 to 0.013mg/kg. In the detection of multiple pesticide residues in milk can meet the requirements of components. This paper provides a simple and practical method for the evaluation of pesticide residues in fresh milk. The method is used to determine fresh milk samples
出处
《生命科学仪器》
2017年第2期54-59,共6页
Life Science Instruments
关键词
气相色谱串联质谱
同时测定
52种农药残留
牛乳
gas chromatography tandem mass spectrometry
simultaneous determination
52 kinds of pesticide residues
milk.
