气相色谱法测定铁皮石斛、浙贝母和人参中嘧菌酯残留  

Determination of Azoxystrobin Residues in Dendrobium officinale,Fritiliariae thunbergii and Panax ginseng by Gas Chromatography

作　　者：范丽丽[1] 王娟[1] 吴加伦[1] 

机构地区：[1]农业部植物病原及昆虫分子生物学重点实验室浙江大学农药与环境毒理研究所,浙江杭州310058

出　　处：《分析科学学报》2017年第2期222-226,共5页Journal of Analytical Science

基　　金：质检公益性行业科研专项(No.20130149)

摘　　要：本文建立了铁皮石斛、浙贝母和人参三种中药材中嘧菌酯的残留检测方法。样品采用乙腈提取,二氯甲烷液-液萃取,弗罗里硅土-中性氧化铝-活性炭柱层析净化,乙酸乙酯定容,气相色谱-电子捕获检测器(GC-ECD)检测,基质外标法定量。结果表明:在0.01~1.0mg/L范围内,不同基质中嘧菌酯的峰面积与其质量浓度间呈良好线性关系,相关系数均大于0.999;在0.01、0.1和0.5mg/kg的添加水平下,嘧菌酯在3种中药材基质中的平均回收率为85.0%~94.9%,日内相对标准偏差(RSD)均小于5.2%(n=5),日间RSD均小于6.7%(n=15);其在铁皮石斛、浙贝母和人参基质中的检出限(LOD)为0.002~0.004mg/kg,定量限(LOQ)均为0.01mg/kg。方法的准确度和精密度均满足残留分析要求,适用于铁皮石斛、浙贝母和人参中嘧菌酯的检测。A method for determination of azoxystrobin residues in Dendrobium officinale,Fritiliariae thunbergii and Panax ginseng was established.Samples were extracted ultrasonically with acetonitrile,partioned by dichloromethane,and then cleaned up by column chromatography（florisil-neutral aluminaactivated charcoal）.The sample extracts were determined by GC-ECD with matrix-matched external standard method.The results indicated that the matrix-matched calibration curves showed good linearity in the concentration range of 0.01-1mg/L with correlation coefficients higher than 0.999.The average recoveries of azoxystrobin in the three matrices were between 85.0% and 94.9% at the spiked levels of 0.01,0.1and 0.5mg/kg,with intra-day relative standard deviations lower than 5.2%（n=5）and interday relative standard deviations lower than 6.7%（n=15）.The limits of detection（LOD）in Dendrobium officinale,Fritiliariae thunbergii and Panax ginseng were 0.002-0.004mg/kg,the limits of quantification（LOQ）were 0.01mg/kg.The method was easy,efficient,sensitive and accurate,which can be suitable for determination of azoxystrobin residues.

关 键 词：嘧菌酯 中药材 气相色谱 残留 

分 类 号：O657.71[理学—分析化学]