气相色谱法测定元胡、浙贝母和白芍中嘧霉胺残留  

Determination of pyrimethanil residue in Corydalis yanhusuo,Fritillaria thunbergii and Paeonia lactiflora by gas chromatography

作　　者：王娟[1] 范丽丽[1] 吴加伦[1] 

机构地区：[1]浙江大学农药与环境毒理研究所,杭州310058

出　　处：《农药学学报》2016年第5期664-668,共5页Chinese Journal of Pesticide Science

基　　金：质检公益性行业科研专项(20130149)

摘　　要：建立了一种测定元胡、浙贝母和白芍3种中药材中嘧霉胺残留的气相色谱分析方法。样品经二氯甲烷提取,液-液分配,柱层析[m（中性氧化铝）：m（弗罗里硅土）=3：2]净化,气相色谱-氮磷检测器（GC-NPD）检测,基质匹配外标法定量,同时经气相色谱-串联质谱（GC-MS/MS）验证。结果表明：在0.02-10 mg/L范围内,分别以正己烷和3种空白基质溶液为溶剂配制嘧霉胺的标准工作溶液,峰面积与相应的质量浓度间呈良好的线性关系,R2均大于0.999;在0.01（元胡中为0.02）、0.1和0.5 mg/kg 3个添加水平下,添加回收率为75%-104%,日内相对标准偏差（RSD）为1.3%-10.2%（n=5）,日间RSD为1.2%-9.0%（n=3）。分析方法在元胡、浙贝母和白芍中的定量限（LOQ）分别为0.02、0.01和0.01 mg/kg。该方法的灵敏度、准确度及精密度均符合农药残留分析要求,且简单易行,净化效果好,适用于元胡、浙贝母和白芍中嘧霉胺分析。A method has been developed for the determination of pyrimethanil residue in Corydalis yanhusuo W.T.Wang,Fritillaria thunbergii Miq.and Paeonia lactiflora Pall.by using gas chromatography.Samples were extracted with dichloromethane,cleaned up by column chromatography（neutral alumina-florisil = 3 ：2,m/m） followed by liquid-liquid partition.Then pesticide residue was determined by gas chromatography with nitrogen-phosphorus detection（NPD）,and the matrix-matched external standard method was applied for the quantitative analysis.The confirmation of pyrimethanil was performed by GC-MS/MS.Good linearity was obtained at concentrations of 0.02-10 mg/L with R2 higher than 0.999 in n-hexane and blank matrix solution.The spiked recoveries varied from 75% to104% at 0.01（0.02 in C.yanhusuo）,0.1,and 0.5 mg/kg spiked levels,respectively.The intra-day relative standard deviation ranged from 1.3% to 10.2%（n = 5） and the inter-day relative standard deviation ranged from 1.2% to 9.0%（n = 3）,in various matrixes.The limit of quantification（LOQ） in C.yanhusuo,F.thunbergii and P.lactiflora was 0.02,0.01,and 0.01 mg/kg,respectively.Thisanalytical method met with the requirement of pesticide residue analysis.It was simple,reliable,and with better purification effect,which could be applied to the determination pyrimethanil residue in these three kinds of Chinese medicinal herbs.

关 键 词：气相色谱 元胡 浙贝母 白芍 嘧霉胺 残留 

分 类 号：S481.8[农业科学—农药学]