气相色谱法测定黄芪中2,2-双(4-氯苯基)-1,1-二氯乙烯  

Determination of 2,2-dichloro-1,1-bis(4-chlorophenyl)ethylene in Astragalus membranaceus by gas chromatography

作　　者：蒲晓亚 郭亮 胡莹莹 宋高林 杨丽娟 PU Xiao-ya;GUO Liang;HU Ying-ying;SONG Gao-lin;YANG Li-juan(Gansu Province Product Quality Inspection East Branch Center,Tianshui 741000,Gansu,China;Tianshui Food Inspection and Testing Center,Tianshui 741000,Gansu,China)

机构地区：[1]甘肃省产品质量监督检验东部分中心,甘肃天水741000 [2]天水市食品检验检测中心,甘肃天水741000

出　　处：《兰州大学学报（自然科学版）》2024年第4期536-541,共6页Journal of Lanzhou University(Natural Sciences)

基　　金：甘肃省科技计划项目(2020GSMPA020)。

摘　　要：建立一种气相色谱条件下有机氯农药残留2,2-双(4-氯苯基)-1,1-二氯乙烯(p,p′-DDE)的检测分析方法.收集8批黄芪样品,采用分析柱、验证柱和加标试验进行分析,通过质谱方法验证干扰物质,在GC-63Ni-ECD条件下成功实现干扰物质的分离和目标成分的测定.p,p′-DDE在1.06~106.09 ng/mL范围的线性关系良好(R=0.9996),阴性样品的回收率为81.31%~88.27%,阳性样品的回收率为75.81%~79.94%.阴性样品的加标溶液在24 h内稳定性良好(相对标准偏差≤3.21%).该方法的检出限为0.21μg/kg,定量限为0.71μg/kg.结果表明,黄芪中存在干扰p,p′-DDE测定的物质,检测过程中应予以高度关注.该检测方法准确、可靠、成本低,可用于黄芪中有机氯农药残留p,p′-DDE的测定.An analytical method was developed under gas chromatographic conditions for the determination of the organochlorine pesticide 2,2-dichloro-1,1-bis(4-chlorophenyl)ethylene(p,p'-DDE)in Astragalus membranaceus samples,eight batches of which were collected and analyzed using an analytical column,validation column and spiked test.Interfering substances were verified using mass spectrometry and successfully separated,and determination of the target component achieved under GC-63Ni-ECD conditions.p,p′-DDE showed a good linear correlation within the range of 1.06 to 106.09 ng/mL(R=0.9996).The recovery rates for negative samples ranged from 81.31%to 88.27%,and for positive samples,ranged from 75.81%to 79.94%.The negative sample spiked solution showed good stability within 24 hours(RSD≤3.21%).The detection limit of this method was 0.21μg/kg,and the quantification limit 0.71μg/kg.The results indicate that,there are substances in A.membranaceus that interfere with the determination of p,p′-DDE,which should be highly noticed during the detection process.The method is accurate,reliable,low-cost,and can be used for the determination of the organochlorine pesticide p,p′-DDE in A.membranaceus.

关 键 词：黄芪 气相色谱法 2 2-双(4-氯苯基)-1 1-二氯乙烯 有机氯农药残留 

分 类 号：R917[医药卫生—药物分析学]