超高效液相色谱-串联质谱法测定凉茶中二十种农药残留的含量
目的 建立QuEChERS结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)测定凉茶中包括霜霉威、多菌灵、噻菌灵等20种农药残留的含量。方法 5.00 mL凉茶经过10.00 mL乙腈提取, QuEChERS法萃取, 经Shim-pack XR-ODS Ⅲ色谱柱分离, 正离子扫描, 多反应监测模式进行质谱分析, 外标法定量。结果 20种农残在1.0~100.0 ng/mL范围内具有良好的线性关系。添加水平为5、10、20 μg/L 时, 方法回收率为75.37%~110.21%, 相对标准偏差均小于13%(n=6), 杀线威、甲萘威、联苯肼酯及噻螨酮的检出限(limits of detection, LODs)为1.0 μg/L, 其余16种农药LODs均 为0.5 μg/L。结论 本研究建立的方法操作简便、快速准确, 适用于凉茶中20种农药残留的快速筛查和定量分析。
Objective To establish a method for the determination of 20 kinds of pesticides residues in herbal tea by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The herbal tea was diluted by 10.00 mL acetonitrile, extracted by QuEChERS method, separated by Shim-pack XR-ODS Ⅲ column, and determined by UPLC-MS/MS with positive electrospray ionization and multiple reaction monitoring (MRM) mode. External standard method was used for quantification. Results The 10 kinds of pesticide residues had good linear relationships in the range of 1.0-100.0 ng/mL. The recoveries were all between 75.32%-110.21% at the spiked levels of 5, 10 and 20 μg/L. The relative standard deviations of the method were less than 13% (n=6). The limits of detection (LODs) of oxamyl, carbaryl, bifenazate and hexythiazox were 1.0 μg/L, and LODs of others were all 0.5 μg/L. Conclusion The established method is simple, accurate and sensitive, which can be used for rapid screening and quantitative analysis of 20 kinds of pesticides in herbal tea.
标题：超高效液相色谱-串联质谱法测定凉茶中二十种农药残留的含量
英文标题：Determination of 20 kinds of pesticide residues in herbal tea by ultra performance liquid chromatography-tandem mass spectrometry
作者：
伍志航 广东产品质量监督检验研究院
梁钰莹 广东产品质量监督检验研究院
何海彤 广东产品质量监督检验研究院
中文关键词:QuEChERS,农药残留,凉茶,超高效液相色谱-串联质谱法,
英文关键词:pesticide residues,herbal tea,ultra performance liquid chromatography-tandem mass spectrometry,
发表日期：2018-03-06
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