QuEChERS-气相色谱-质谱联用法快速测定人参中农药多残留
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摘要
建立了QuEChERS-气相色谱-质谱联用(GC-MS)法同时测定人参中20种农药残留量的检测技术。样品前处理采用改进的QuEChERS方法,人参粉加水浸润后,用乙腈均质提取,用N-丙基乙二胺(PSA)和MgSO_4净化,结合GC-MS检测系统,在电子轰击源(EI)选择离子监测(SIM)模式下进行检测,使用HP-5毛细管柱进行分离。在优化条件下, 20种农药在一定范围内线性关系良好,相关系数大于0. 990,方法检出限(信噪比S/N=3)为0. 001～0. 007 mg/kg,定量限(S/N=10)为0. 002～0. 024 mg/kg,平均回收率为70. 41%～114. 06%,相对标准偏差(RSD)为0. 76%～15. 47%。该方法操作简单快捷、灵敏度高。
In this study,the extraction and purification improvements of the QuEChERS method were coupled with gas chromatography-mass spectrometry( GC-MS) to determine 20 pesticides in panax ginseng. Dry ginseng powder was mixed with water,and the solution was then extracted with acetonitrile and purified with N-propylethylenediamine( PSA) and MgSO4 to remove co-extractives that might interfere with the results. The target compounds were detected after electron-impact ionization in selected ion monitoring( SIM) mode. Under optimum conditions,the method gave a good linear relationship for the determination of the pesticides within a certain concentration range,with correlation coefficients greater than 0. 990. Moreover,the limits of detection( S/N = 3) were 0. 002-0. 007 mg/kg,the limits of quantification( S/N = 10)were 0. 002-0. 024 mg/kg,and the average recoveries for pesticides in panax ginseng were70. 41%-114. 06%,with relative standard deviations of 0. 76%-15. 47%. In comparison with previous methods,the newprocedure has the advantages of simple sample preparation and higher sensitivity.
In this study,the extraction and purification improvements of the QuEChERS method were coupled with gas chromatography-mass spectrometry( GC-MS) to determine 20 pesticides in panax ginseng. Dry ginseng powder was mixed with water,and the solution was then extracted with acetonitrile and purified with N-propylethylenediamine( PSA) and MgSO4 to remove co-extractives that might interfere with the results. The target compounds were detected after electron-impact ionization in selected ion monitoring( SIM) mode. Under optimum conditions,the method gave a good linear relationship for the determination of the pesticides within a certain concentration range,with correlation coefficients greater than 0. 990. Moreover,the limits of detection( S/N = 3) were 0. 002-0. 007 mg/kg,the limits of quantification( S/N = 10)were 0. 002-0. 024 mg/kg,and the average recoveries for pesticides in panax ginseng were70. 41%-114. 06%,with relative standard deviations of 0. 76%-15. 47%. In comparison with previous methods,the newprocedure has the advantages of simple sample preparation and higher sensitivity.
引文
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[35] EN 15662-2008
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[5] Jilin Province Office of Ginseng and Antler. Agrochemicals,2014(2):39吉林省参茸办.农药,2014(2):39
[6] Liu D J,Xue J,Cui C. China Journal of Chinese Materia Medica,2008,33(20):2421刘东静,薛健,崔澈.中国中药杂志,2008,33(20):2421
[7] He M.[MS Dissertation]. Yanji:Yanbian University,2009:35何苗.[硕士学位论文].延吉:延边大学,2009:35
[8] Peng F.[MS Dissertation]. Beijing:Peking Union Medical Co llege,2008:59彭非.[硕士学位论文].北京:中国协和医科大学,2008:59
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[11] Luo J,Wang Y F,Jin C A,et al. Special Wild Economic Anim al and Plant Research,2013(4):58罗婧,王玉方,金春爱,等.特产研究,2013(4):58
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[29] Bai B Q,Li M P,Zhang S W. Food Science,2014,35(24):254白宝清,李美萍,张生万.食品科学,2014,35(24):254
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[34] Association of Official Analytical Chemists. Pesticide Residues in Fo o ds by Aceto nitrile Ex tractio n and Partitio ning w ith Magnesium Sulfate.[2018-04-12]. http://w w w. eo m a.ao ac.o rg/m etho ds/info.asp?ID=48938
[35] EN 15662-2008
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