首页|气相色谱法测定黄芪中2,2-双(4-氯苯基)-1,1-二氯乙烯

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

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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=0.999 6),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0.21 μg/kg,定量限为0.71 µg/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 determi-nation 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 analyti-cal column,validation column and spiked test.Interfering substances were verified using mass spectrome-try and successfully separated,and determination of the target component achieved under GC6Ni-ECD conditions.p,p'-DDE showed a good linear correlation within the range of 1.06 to 106.09 ng/mL(R=0.999 6).The recovery rates for negative samples ranged from 81.31%to 88.27%,and for positive sam-ples,ranged from 75.81%to 79.94%.The negative sample spiked solution showed good stability with-in 24 hours(RSD≤3.21%).The detection limit of this method was 0.21 μg/kg,and the quantification limit 0.71 μg/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.

Astragalus membranaceusgas chromatography2,2-dichloro-1,1-bis(4-chlorophenyl)ethyl-eneinorganochlorine pesticide residue

蒲晓亚、郭亮、胡莹莹、宋高林、杨丽娟

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甘肃省产品质量监督检验东部分中心,甘肃天水 741000

天水市食品检验检测中心,甘肃天水 741000

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

2024

兰州大学学报(自然科学版)
兰州大学

兰州大学学报(自然科学版)

CSTPCD北大核心
影响因子:0.855
ISSN:0455-2059
年,卷(期):2024.60(4)