分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留  

Simultaneous Determination of Triazine Pesticides in Honey by Using UHPLC-HRMS Combined with DSPE

作　　者：何丽君[1] 陈豪[1] 翁淑琴[1] 郑婉玉[1] 严国鸿[1] 胡敏 李德森[3] 

机构地区：[1]福建中医药大学附属人民医院,福州350004 [2]福建省食品药品质量检验研究院,福州350003 [3]福建中医药大学,福州350122

出　　处：《中国实验方剂学杂志》2016年第22期71-76,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：福建省科技厅社发处重点项目(2014Y0060);全国中药特色技术传承人才培训项目(J20164811007)

摘　　要：目的：采用分散固相萃取技术（DSPE）,建立蜂蜜中21种三嗪类农药残留的同时测定分析方法。方法：用15%氯化钠水溶液溶解蜂蜜后,以1%甲酸乙腈进行盐析提取,提取液经DSPE净化后,采用超高效液相色谱-高分辨质谱（UHPLCHRMS）进行外标法定量检测。结果：21种三嗪类农药在各自浓度范围内具有较好的线性相关系数（r〉0.999）。目标化合物在低、中、高3个浓度下的平均回收率为73.9%~110.4%（RSD 1.5%~9.6%）,定量限（LOQ）为1~10μg·kg-1。结论：该方法灵敏度高、准确性好,适合蜂蜜样品中21种三嗪类农药的快速准确定量分析。Objective： To develop a method for the simultaneous determination of 21 triazine pesticides in honey by using dispersive solid phase extraction（DSPE）. Method： Honey samples were dissolved in 15% Na Cl solution and extracted with 1% formic acid in acetonitrile by salting out method. The extracts were purified by DSPE procedure,and the quantitative analysis was operated by ultra high performance liquid chromatography- high resolution mass spectrometry（UHPLC-HRMS）. Result： 21 traizine pesticides showed good linearity within their respective concentration range（r〉 0. 999）. The average recovery rates were 73. 9%-110. 4%（RSD 1. 5%-9. 6%） under low,middle and high concentrations,and the LOQs were from 1 to 10 μg·kg- 1. Conclusion： The proposed method was sensitive and accurate,which was suitable for the rapid simultaneous determination of 21 triazine pesticide residues in honey.

关 键 词：蜂蜜 三嗪类农药 分散固相萃取 超高效液相色谱-高分辨质谱 

分 类 号：R284.1[医药卫生—中药学]