在线凝胶渗透色谱-气相色谱质谱联用仪测定药食同源样品中30种农药残留
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摘要
目的建立药食同源食品中多种农药残留检测的在线凝胶渗透色谱-气相色谱-质谱联用法(gel permeation chromatography-gas chromatography-mass spectrometry, GPC-GC-MS)。方法本研究采用3种不同净化方式对药食同源样品进行前处理,利用在线凝胶渗透色谱-气相色谱质谱联用仪测定样品中30种农药残留。结果结果表明30种农药在0.01～0.2μg/mL浓度范围内线性关系良好,检出限为0.01 mg/kg,药食同源样品3个水平添加回收为69.1%～88.8%,相对标准偏差为3.3%～19.4%。结论3种方法中QuEChERS法灵敏度高,准确性好,可用于药食同源样品中多种农药残留的同时测定。
Objective To establish a method for determination of pesticide residues in homologous samples of medicines and foods by gel permeation chromatography-gas chromatography-mass spectrometry(GPC-GC-MS).Methods Three different purification methods were used for pretreatment of homologous samples of medicines and foods. Thirty kinds of pesticide residues in the samples were determined by GPC-GC-MS. Results The results showed that 30 kinds of pesticides had good linear relationships in the range of 0.01-0.2 μg/mL, the limits of detection were 0.01 mg/kg, and the recoveries at 3 spiked levels of the three added levels of the homologous samples of medicines and foods samples were 69.1%-88.8%, with the relative standard deviations of 3.3%-19.4%. Conclusion Among the three methods, QuEChERS method has high sensitivity and accuracy, which can be used for simultaneous determination of multiple pesticide residues in the homologous samples of medicines and foods.
Objective To establish a method for determination of pesticide residues in homologous samples of medicines and foods by gel permeation chromatography-gas chromatography-mass spectrometry(GPC-GC-MS).Methods Three different purification methods were used for pretreatment of homologous samples of medicines and foods. Thirty kinds of pesticide residues in the samples were determined by GPC-GC-MS. Results The results showed that 30 kinds of pesticides had good linear relationships in the range of 0.01-0.2 μg/mL, the limits of detection were 0.01 mg/kg, and the recoveries at 3 spiked levels of the three added levels of the homologous samples of medicines and foods samples were 69.1%-88.8%, with the relative standard deviations of 3.3%-19.4%. Conclusion Among the three methods, QuEChERS method has high sensitivity and accuracy, which can be used for simultaneous determination of multiple pesticide residues in the homologous samples of medicines and foods.
引文
[1]杨银慧,豆小文,孔维军,等.我国中药材中农药登记现状及污染分析[J].中国中药杂志,2013,38(24):4238.Yang YH, Dou XW, Kong WJ, et al. Status of pesticide registration and pollution in Chinese herbal medicines[J]. J Tradit Chin Med, 2013, 38(24):4238.
[2]康传志,郭兰萍,周涛,等.中药材农残研究现状的探讨[J].中国中药杂志,2016,41(2):155-59.Kang CZ, Guo LP, Zhou T, et al. Discussion on the status quo of research on pesticide residues in traditional Chinese medicine[J]. J Tradit Chin Med, 2016, 41(2):155-59.
[3]李春艳.QuEChERS法-色质联用技术在农药残留检测应用中的研究[D].西安:西安理工大学,2010.Li CY. Study on QuEChERS method in the application of chromatography-mass spectrometry in pesticide residue detection[D].Xi'an:Xi'an University of Technology, 2010.
[4]俞芳,贾丽娟,黄薇,等.中药材农药残留分析中的前处理方法比较[J].农药,2014,53(9):666-669.Yu F, Jia LJ, Huang W, et al. Comparison of pretreatment methods in analysis of pesticide residues in Chinese herbal medicines[J].Agrochemicals, 2014,53(9):666-669.
[5]钟瑶.不同中药制剂中有机农药多残留分析新技术研究[D].南昌:南昌大学,2014.Zhong Y. Study on new technology of multi-residue analysis of organic pesticide in different traditional chinese medicine preparations[D].Nanchang:Nanchang University, 2014.
[6]翁淑琴.桔梗等药材中拟除虫菊酯和有机磷农药残留的分析研究[D].福建:福建医科大学,2006.Weng SQ. Analysis of pyrethroid and organophosphorus pesticide residues in platycodon and other medicinal materials[D]. Fujian:Fujian Medical University, 2006.
[7]黄晓会,薛健,吴晓波,等.根茎类中药材有机氯及菊酯类农药多残留分析[J].中成药,2012, 34(1):100-104.Huang XH, Xue J, Wu XB, et al. Multi-Residue analysis of organochlorine and pyrethroid pesticides in rhizome Chinese herbal medicines[J]. Chin Tradit Pat Med, 2012, 34(1):100-104.
[8]钟冬莲.铁皮石斛中农药多残留检测技术及应用研究[D].杭州:浙江工业大学,2017.Zhong DL. Detection technology and application of pesticide residues in Dendrobium candidum[D]. Hangzhou:Zhejiang University of Technology,2017.
[9]范保瑞,张悦,刘红玉,等.国内药食同源的产生与应用[J].医学研究与教育,2018, 35(6):52-64.Fan BR, Zhang R, Liu HY, et al. The generation and application of domestic medicine and food homology[J]. Med Res Edu, 2018, 35(6):52-64.
[10]蒋军辉,徐小娜,于军晖,等.气相色谱-质谱联用技术分析藿香挥发油化学成分[J].南华大学学报(自然科学版),2016, 30(1):77-81.Jiang YH, Xu XN, Yu JH, et al. Analysis of chemical constituents of volatile oil from musk by gas chromatography-mass spectrometry[J]. J Nanhua Univ(Nat Sci Ed), 2016, 30(1):77-81.
[11]吴宁华,杨敏,雷咪,等.中草药中拟除虫菊酯类农药残留的顶空-固相微萃取方法考察[J].湖北中医药大学学报,2012, 14(3):35-37.Wu NH, Yang M, Lei M, et al. Headspace-solid phase microextraction method for pyrethroid pesticide residues in Chinese herbal medicine[J]. J Hubei Univ Tradit Chin Med, 2012, 14(3):35-37.
[12]蒋玉宝,刘筱,张丽萍,等.甘肃省枸杞农药残留状况及出口风险分析[J].甘肃农业科技,2019,(1):37-42.Jiang YB, Liu Y, Zhang LP, et al. Analysis of pesticide residues and export risks in Gansu province[J]. Gansu Agric Sci Technol, 2019,(1):37-42.
[13]马桂娟,张瑶,汤丽华,等.GC-MS/MS同时测定枸杞籽油中28种农药残留[J].中国酿造,2019, 38(2):194-198.Ma GJ, Zhang Y, Tang LH, et al. Simultaneous determination of 28pesticide residues in alfalfa seed oil by GC-MS/MS[J]. China Brew, 2019,38(2):194-198.
[14]陈蕾.固相萃取技术在中药分析中的应用[J].中国药事,2012, 26(2):159-161.Chen L. Application of solid phase extraction technology in analysis of traditional Chinese medicine[J] Chin Pharm Aff, 2012, 26(2):159-161.
[15]修丽华.固相萃取气相色谱法测定中药材中有机氯及拟除虫菊酯类农药残留[D].长春:吉林大学,2005.Xiu LH. Determination of organochlorine and pyrethroid pesticide residues in traditional Chinese medicine by solid phase extraction and gas chromatography[D]. Changchun:Jilin University, 2005.
[16] SN/T 1957-2007进出口中药材及其制品中五氯硝基苯残留量检测方法气相色谱-质谱法[S].SN/T 1957-2007 Methods for the determination of the residues of pentachloronitrobenzene in imported and exported Chinese medicinal materials and their products-Gas chromatography-mass spectrometry[S].
[17] GB 23200.10-2016食品安全国家标准桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法[S].GB 23200.10-2016 National food safety standard-Determination of residues of 488 pesticides and related chemicals in mulberry branch,honeysuckle, medlar fruit and lotus leaf-Gas chromatography-mass spectrometry[S].
[2]康传志,郭兰萍,周涛,等.中药材农残研究现状的探讨[J].中国中药杂志,2016,41(2):155-59.Kang CZ, Guo LP, Zhou T, et al. Discussion on the status quo of research on pesticide residues in traditional Chinese medicine[J]. J Tradit Chin Med, 2016, 41(2):155-59.
[3]李春艳.QuEChERS法-色质联用技术在农药残留检测应用中的研究[D].西安:西安理工大学,2010.Li CY. Study on QuEChERS method in the application of chromatography-mass spectrometry in pesticide residue detection[D].Xi'an:Xi'an University of Technology, 2010.
[4]俞芳,贾丽娟,黄薇,等.中药材农药残留分析中的前处理方法比较[J].农药,2014,53(9):666-669.Yu F, Jia LJ, Huang W, et al. Comparison of pretreatment methods in analysis of pesticide residues in Chinese herbal medicines[J].Agrochemicals, 2014,53(9):666-669.
[5]钟瑶.不同中药制剂中有机农药多残留分析新技术研究[D].南昌:南昌大学,2014.Zhong Y. Study on new technology of multi-residue analysis of organic pesticide in different traditional chinese medicine preparations[D].Nanchang:Nanchang University, 2014.
[6]翁淑琴.桔梗等药材中拟除虫菊酯和有机磷农药残留的分析研究[D].福建:福建医科大学,2006.Weng SQ. Analysis of pyrethroid and organophosphorus pesticide residues in platycodon and other medicinal materials[D]. Fujian:Fujian Medical University, 2006.
[7]黄晓会,薛健,吴晓波,等.根茎类中药材有机氯及菊酯类农药多残留分析[J].中成药,2012, 34(1):100-104.Huang XH, Xue J, Wu XB, et al. Multi-Residue analysis of organochlorine and pyrethroid pesticides in rhizome Chinese herbal medicines[J]. Chin Tradit Pat Med, 2012, 34(1):100-104.
[8]钟冬莲.铁皮石斛中农药多残留检测技术及应用研究[D].杭州:浙江工业大学,2017.Zhong DL. Detection technology and application of pesticide residues in Dendrobium candidum[D]. Hangzhou:Zhejiang University of Technology,2017.
[9]范保瑞,张悦,刘红玉,等.国内药食同源的产生与应用[J].医学研究与教育,2018, 35(6):52-64.Fan BR, Zhang R, Liu HY, et al. The generation and application of domestic medicine and food homology[J]. Med Res Edu, 2018, 35(6):52-64.
[10]蒋军辉,徐小娜,于军晖,等.气相色谱-质谱联用技术分析藿香挥发油化学成分[J].南华大学学报(自然科学版),2016, 30(1):77-81.Jiang YH, Xu XN, Yu JH, et al. Analysis of chemical constituents of volatile oil from musk by gas chromatography-mass spectrometry[J]. J Nanhua Univ(Nat Sci Ed), 2016, 30(1):77-81.
[11]吴宁华,杨敏,雷咪,等.中草药中拟除虫菊酯类农药残留的顶空-固相微萃取方法考察[J].湖北中医药大学学报,2012, 14(3):35-37.Wu NH, Yang M, Lei M, et al. Headspace-solid phase microextraction method for pyrethroid pesticide residues in Chinese herbal medicine[J]. J Hubei Univ Tradit Chin Med, 2012, 14(3):35-37.
[12]蒋玉宝,刘筱,张丽萍,等.甘肃省枸杞农药残留状况及出口风险分析[J].甘肃农业科技,2019,(1):37-42.Jiang YB, Liu Y, Zhang LP, et al. Analysis of pesticide residues and export risks in Gansu province[J]. Gansu Agric Sci Technol, 2019,(1):37-42.
[13]马桂娟,张瑶,汤丽华,等.GC-MS/MS同时测定枸杞籽油中28种农药残留[J].中国酿造,2019, 38(2):194-198.Ma GJ, Zhang Y, Tang LH, et al. Simultaneous determination of 28pesticide residues in alfalfa seed oil by GC-MS/MS[J]. China Brew, 2019,38(2):194-198.
[14]陈蕾.固相萃取技术在中药分析中的应用[J].中国药事,2012, 26(2):159-161.Chen L. Application of solid phase extraction technology in analysis of traditional Chinese medicine[J] Chin Pharm Aff, 2012, 26(2):159-161.
[15]修丽华.固相萃取气相色谱法测定中药材中有机氯及拟除虫菊酯类农药残留[D].长春:吉林大学,2005.Xiu LH. Determination of organochlorine and pyrethroid pesticide residues in traditional Chinese medicine by solid phase extraction and gas chromatography[D]. Changchun:Jilin University, 2005.
[16] SN/T 1957-2007进出口中药材及其制品中五氯硝基苯残留量检测方法气相色谱-质谱法[S].SN/T 1957-2007 Methods for the determination of the residues of pentachloronitrobenzene in imported and exported Chinese medicinal materials and their products-Gas chromatography-mass spectrometry[S].
[17] GB 23200.10-2016食品安全国家标准桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法[S].GB 23200.10-2016 National food safety standard-Determination of residues of 488 pesticides and related chemicals in mulberry branch,honeysuckle, medlar fruit and lotus leaf-Gas chromatography-mass spectrometry[S].
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