[目的]通过选取适宜的分析色谱柱,简化样品的前处理过程,选取合适的离子对进行监测,提高方法的灵敏度和准确度。[方法]测定样品平行性（精密度）、加标回收率（准确度）、方法检出限,对该检测方法进行验证。[结果]牛奶中添加甲基毒死蜱的回收率分别为105.3%、106.9%、108.2%,甲基毒死蜱在3 个添加水平上的变异系数分别为1.61%、3.06%、2.52%。奶粉中添加甲基毒死蜱的回收率分别为100.3%、89.8%、88.5%,甲基毒死蜱在3 个添加水平上的变异系数分别为2.14%、1.97%、1.82%。[结论]该方法精密度和准确度符合要求,可用于牛奶和奶粉中日常甲基毒死蜱残留的测定和质量控制。
赵凤茹, 谢凯丽, 水明, 丛慧敏, 薛文强, 李琪琪, 代晶晶, 龙洋, 王婼依
. 测定牛奶和奶粉中甲基毒死蜱残留量的气相色谱串联质谱法研究[J]. 中国乳业, 2025
, 0(4)
: 97
-103
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DOI: 10.12377/1671-4393.25.04.17
[Objective] By selecting the appropriate analytical chromatographic column,the pretreatment process of the sample was simplified,and the suitable ion pairs were selected for monitoring,the sensitivity and accuracy of the method were improved. [Method] The parallelism （precision）of the samples,the recovery rate of spiked samples（accuracy）,and the detection limit of the method were determined to verify the detection method. [Result] The recovery rates of methyl chlorpyrifos added to milk were 105.3%,106.9% and 108.2%,and the coefficients of variation at the three addition levels were 1.61%,3.06% and 2.52%. The recovery rate of methyl parathion added to milk powder were 100.3%,89.8% and 88.5%,and the coefficients of variation at the three addition levels were 2.14%,1.97% and 1.82%. [Conclusion] The precision and accuracy of this method met the requirements and it could be used for the determination and quality control of daily methyl chlorpyrifos residues in milk and milk powder.
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