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固相萃取-在线凝胶渗透色谱-气相色谱/质谱法测定松子仁中的28种有机氯农药和拟除虫菊酯农药
Determination of 28 organochlorine and pyrethroid pesticides in pine nuts using solid-phase extraction and on-line gel permeation chromatography-gas chromatography/mass spectrometry
【摘要】 建立了松子仁中28种有机氯农药和拟除虫菊酯农药多残留的在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析方法。样品以乙腈-水(体积比为4∶1)为提取剂高速匀浆提取,提取液经Aluminium-N固相萃取柱净化,除去样品中大部分的脂肪和甾醇等干扰基质,再经在线GPC进一步除去样液中的色素和脂肪等大分子干扰物质,有效地降低了样品复杂基质带来的背景干扰。加标水平为0.05mg/kg时,大部分农药的回收率为70%~120%,相对标准偏差小于15%。28种农药的检出限为0.002~0.05mg/kg。采用外标法定量,方法的线性关系和回收率结果均令人满意。实验证明,该方法是一种快速、准确、灵敏度高的同时检测松子仁中农药多残留的检测方法。
【Abstract】 An analytical method has been developed for the determination of 28 organochlorine pesticides and pyrethroid pesticides in pine nuts.The sample was extracted With acetonitrile-water(4∶1,v/v) as the extraction solution by means of high-speed homogenization.The crude extract was purified by an Aluminium-N solid phase extraction column to remove most of the fat and sterols in the sample,then on-line gel permeation chromatography-gas chromatography/mass spectrometry(GPC-GC/MS) analysis was performed.The recoveries for the most of pesticides in the sample spiked with the standards of 0.05 mg/kg were 70%-120%,and the relative standard deviations were less than 15%.The limits of detection of 28 organochlorine pesticides and pyrethroid pesticides were 0.002-0.05 mg/kg.The linear relationship and the recovery results were satisfactory.The method is rapid,accurate,highly senstive,and can be used for the simultaneous determination of pesticide residues in pine nuts.
【Key words】 solid-phase extraction(SPE); on-line gel permeation chromatography-gas chromatography/mass spectrometry(GPC-GC/MS); organochlorine pesticides; pyrethroid pesticides; pine nuts;
- 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2009年02期
- 【分类号】TS255.7
- 【被引频次】62
- 【下载频次】653