目的 建立基于气相色谱-串联质谱法(GC-MS/MS)麦冬中56种农药残留量的快速检测方法,并应用于137批样品筛查。方法 选择禁限用及常用农药作为检测指标。采用QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)法对样品进行前处理,在气相色谱-串联质谱多反应监测模式(MRM)下进行测定,以3个添加水平测定样品的回收率和RSD。结果 56种农药在一定含量范围内线性关系良好,相关系数(r)均大于0.997 8;在LOD、2 LOD、10 LOD 3个添加浓度水平进行回收率实验中,96.4%的农药在60%~130%内,92.9%的农药RSD小于15%;绝大多数农药检测限小于0.01 mg·kg-1。137批麦冬中共检出12种农药。结论 该方法检测指标具有一定针对性,且操作简便快速、灵敏可靠,适用于麦冬中农药残留的筛查测定。试验结果对于麦冬的生产种植和流通监管具有一定的参考意义。
Abstract
OBJECTIVE To establish a method for simultaneous determination of 56 kinds of pesticide residues in Radix Ophiopogonis by using gas chromatography tandem mass spectrometry (GC-MS/MS), and apply it to screening of 137 batches of samples. METHODS The forbidden, restricted and frequently-used pesticides were selected as the detecting indexes. The samples were prepared by QuEChERS, and quantitative analysis was carried out by GC-MS/MS in multiple-reaction monitoring (MRM)mode. There were three supplemental levels for detection recoveries and RSD. RESULTS All the 56 pesticides had good linearity in certain ranges with correlation coefficients(r) higher than 0.997 8. The recoveries of 96.4% pesticides ranged from 60% to 130% at three supplemental levels (1, 2 and 10 LODs), with the RSDs of 92.9% pesticides less than 15%. The LODs for most of the selected pesticides were below 0.01 mg·kg-1. Twelve pesticides were detected in 137 batches of samples. CONCLUSION The detecting indexes are meaningful and the developed method is simple, rapid, sensitive and reliable for screening multiple pesticide residues in Radix Ophiopogonis. The test result has certain reference value for the cultivation and distribution supervision of Radix Ophiopogonis.
关键词
麦冬 /
农药残留 /
气相色谱-串联质谱法 /
QuEChERS法
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Key words
Radix Ophiopogonis /
pesticide residue /
GC-MS/MS /
QuEChERS
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中图分类号：
R284
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参考文献
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脚注
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基金
药品医疗器械审评审批制度改革子课题(中药)项目资助(ZG2016-2-05)
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