凝胶渗透色谱净化-气相色谱-质谱法同时测定金银花中33种农药残留组分

Determination of 33 Pesticide Residues in Honeysuckle by Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry

建立了凝胶渗透色谱(GPC)净化、气相色谱-质谱(GC-MS)同时测定金银花中33种有机氯、有机磷和拟除虫菊酯农药残留的方法。样品中的待测农药组分经乙酸乙酯-环己烷混合溶剂(1∶1,V/V)提取、GPC净化去除色素等杂质,GC-MS采用全扫描/选择离子监测模式(Scan/SIM)采集数据后进行定性/定量分析。方法的相对标准偏差(RSD)≤16.70%(6.9～84.6ng/g,n=5);5种不同加标浓度下,待测农药的标准加入回收率在57.4%(甲胺磷)～109.9%(马拉硫磷)之间;各农药组分的定性检出限(3σ)为0.10～10.5ng/g,定量检出限(10σ)为0.33～20.0ng/g。

A method was developed for the simultaneous determination of 33 pesticide residues, including organochlorine, organophosphorus and pyrethroid pesticide, in honeysuckle by gel permeation chromatography（GPC） purification and gas chromatography-mass spectrometry（GC-MS） detection. The pesticides were extracted using mixed solvent of ethyl-acetate and cyclohexane（1∶1, V/V）. The pesticides extracted from sample were separated and purified with matrices such as pigment by gel permeation chromatography. The pesticides were finally separated and detected by GC-MS with full scan and selective ion monitor mode simultaneously. The precisions of developed method with relative standard deviation for 33 pesticide were lower than 16.7%（6.9-84.6 ng/g, n=5）. The recoveries for 33 pesticide standards spiked samples were between 57.4%（methamidophos） and 109.9%（malathion）. Limits of detection（3σ） and quantifications（10σ） of the method were 0.10-10.5 ng/g and 0.33-20.0 ng/g, respectively.