摘要
目的优化前处理操作,避免样品的前处理问题影响最终定量结果的准确性。方法比较分析了牛奶中农药残留测定的前处理过程中移液器的使用、药品的加入量、样品的提取、样品的浓缩程度、旋转蒸发瓶的选择、样品的洗涤提取、样品的净化等操作步骤,对色谱图中杂质及加标回收率的影响。结果规范优化前处理过程后,平均回收率由75.43%提高至92.64%,平行样的相对标准偏差由8.48%降低至2.02%,减少了杂质对样品的影响。结论该方法前处理优化后,检测方法更为准确、有效,适合测定牛奶中的有机氯类农药残留。
Objective To optimize the pre-processing operation to avoid the problem of sample pre-processing affecting the accuracy of the final quantitative results.Methods The influence of the operation steps such as the use of pipettes,the amount of drugs added,the extraction of samples,the degree of sample concentration,the selection of rotary evaporation bottles,the washing and extraction of samples,and the purification of samples on the impurities in chromatogram and recoveries of spiked were compared and analyzed.Results After the optimization of the pretreatment process,the average recovery rate increased from 75.43%to 92.64%,and the relative standard deviation of the parallel samples was reduced from 8.48%to 2.02%,which reduced the impact of impurities on the samples.Conclusion After the optimization of the pretreatment method,the detection method is more accurate and effective,which is suitable for the determination of organochlorine pesticide residues in milk.
作者
王争争
郭明刚
范丽丽
王艳飞
张云鲜
杨云
WANG Zheng-Zheng;GUO Ming-Gang;FAN Li-Li;WANG Yan-Fei;ZHANG Yun-Xian;YANG Yun(Mengniu Dairy Industry(Jiaozuo)Co.,Ltd,Jiaozuo 454000,China)
出处
《食品安全质量检测学报》
CAS
2020年第5期1390-1399,共10页
Journal of Food Safety and Quality
关键词
有机氯类农药
前处理
牛奶
organochlorine pesticides
pretreatment
milk