摘要
目的:评估液态乳中农药残留量的安全性。方法:建立同时测定11种农药残留的超高效液相色谱—串联质谱法。待测样品经乙腈提取,C18和PSA固相萃取剂净化,经色谱柱Xbridge BEH C18(100 mm×2.1 mm, 1.7μm)分离,多反应监测模式进行测定,并使用响应曲面法优化前处理参数。结果:前处理的最佳条件为乙腈用量10 mL,C18用量50 mg, PSA用量30 mg。11种农药在1.0~100.0μg/L的浓度范围内线性关系良好,相关系数(R2)均>0.999。在10,20,100μg/kg添加水平内,11种农药的平均回收率为82.7%~102.0%,相对标准偏差为2.89%~8.87%,检出限和定量限分别为2.0~3.0,5.0~10.0μg/kg。结论:该方法操作简便,分析时间短,回收率高,重现性好,能够准确定性定量分析液态乳中11种农药残留量。
Objective:This study aimed to evaluate the safety of pesticide residues in liquid milk.Methods:A method for simultaneous determination of 11 kinds of pesticide residues by ultra-high-performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted by acetonitrile,purified by C 18 and PSA solid phase extractants,separated on a column Xbridge BEH C 18(100 mm×2.1 mm,1.7μm),determined in multi-reaction monitoring mode,and optimized for pre-treatment parameters using response surface method.Results:The optimal conditions for pretreatment were 10 mL acetonitrile,50 mg C 18 and 30 mg PSA.The linear relationships of 11 kinds of pesticides were good in the concentration range of 1.0~100.0μg/L,and the correlation coefficients(R 2)were all>0.999.With addition of 10,20,100μg/kg,the average recoveries were 82.7%~102.0%,the relative standard deviations were 2.89%to 8.87%,and the limits of detection(LOD)and limits of quantitation(LOQ)were 2.0~3.0μg/kg and 5.0~10.0μg/kg,respectively.Conclusion:The method is simple,convenient,rapid,high recovery rate and high reproducibility,which could accurately determine 11 kinds of pesticide residues in liquid milk.
作者
黄曼谷
罗永浩
严婉盈
许丽珠
HUANG Mangu;LUO Yonghao;YAN Wanying;XU Lizhu(Guangzhou Inspection Testing and Certification Group Co.,Ltd.,Guangzhou,Guangdong 511447,China;National Quality Inspection and Testing Center for Processed Foods〔Guangdong〕,Guangzhou,Guangdong 511447,China)
出处
《食品与机械》
CSCD
北大核心
2023年第12期48-54,87,共8页
Food and Machinery
基金
广州市市场监督管理局科技项目(编号:2022kj49)。
