固相萃取/GC/MS测定金银花中有机磷农药残留量

何笑荣;邹定;冯金红;吴学军;胡欣;孙春华

中国药学杂志 ›› 2007, Vol. 42 ›› Issue (24) : 1901-1904.

中国药学杂志 ›› 2007, Vol. 42 ›› Issue (24) : 1901-1904.
论著

固相萃取/GC/MS测定金银花中有机磷农药残留量

  • 何笑荣;邹定;冯金红;吴学军;胡欣;孙春华
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Determination of Organophosphorus Pesticides in Flos Lonicerae Japonicae by SPE GC/MS

  • HE Xiao-rong1,ZOU Ding1,FENG Jin-hong2,WU Xue-jun1,HU Xin1,SUN Chun-hua1
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摘要

目的建立固相萃取/GC/MS测定金银花中14种有机磷农药残留的方法。方法样品用冰浴超声提取,Florisil固相萃取小柱(500 mg)加0.2 g活性炭净化提取液。采用GC/MS全扫描(Full Scan)与标准谱库的谱图匹配比较定性,选择离子模式(SIM)定量。结果14种有机磷农药的峰面积与其质量浓度均有良好的线性关系,其相关系数在0.980 2~1.000 0,最低检测限为0.017 9~0.092 5 ppm(S/N=3),加样品回收率在65.02%~107.04%,RSD为3.6%~8.0%。结论本法简便快速,灵敏度高,为其他中药中有机磷农药残留的检测提供参考。

Abstract

OBJECTIVE To establish an analytical method for the determination of 14 kinds of organophosphate pesticide residues in Flos Lonicerae Japonicae by solid-phase extraction(SPE) and Gas Chromatograph-mass spectrometry.METHODS Ultrasonication with acetone in ice bath was used for sample preparation.The sample was processed by SPE column added with 0.2 g active carbon.The total ion current(TIC)was identified with a spectrum library search.Selected ion monitoring(SIM)was used as quantify.RESULTS All the organophosphate pesticide showed good linearity in a detected concentration range with good correlation coefficient(r=0.980 2~1.000 0).The method recoveries were generally 65.02%~107.04% with RSD 3.6%~8.0% and the limit of detection was 0.017 9~0.092 5 ppm(S/N =3).CONCLUSION The method is effective,fast,accurate and provide an analytical method of the organophosphate pesticide residue in traditional medicine.

关键词

金银花 / 有机磷农药残留 / 气相色谱-质谱法 / 固相萃取

Key words

Lonicera chrysantha / organophosphorus pesticides residues / GC-MS

引用本文

导出引用
何笑荣;邹定;冯金红;吴学军;胡欣;孙春华. 固相萃取/GC/MS测定金银花中有机磷农药残留量[J]. 中国药学杂志, 2007, 42(24): 1901-1904
HE Xio-rong;ZOU Ding;FENG Jin-hong;WU Xue-jun;HU Xin;SUN Chun-hu. Determination of Organophosphorus Pesticides in Flos Lonicerae Japonicae by SPE GC/MS [J]. Chinese Pharmaceutical Journal, 2007, 42(24): 1901-1904

参考文献

[1] GE Z R.Maximum Residue Limits of Agricultural Chemicals in Foods Volume of Agricultural Chemicals(食品中农业化学品残留限量)[M] .Beijing:China Standard Press,2006. [2] LONG S,ZHOU Y G,WANG X C,et al. Solid phase extraction GC analysis of organic phosphorus insecticide in rice[J] . Practi Prev Med(实用预防医学),2001,8(5):341-342. [3] Ch.P(2005)VolⅠ(中国药典2005年版一部)[S] .2005:53. [4] FENG X Q,TANG Q Y.Multiresidue determination of organophorous pesticides in Chinese medicinal herbs[J] .Pestic Sci Mange(农药科学与管理),2002,23(2):17-20. [5] XIANG Z X,ZHAO W J,GAO S L.Determination of 11 kinds of organophosphate pesticide residue in Flos Lonicerae by solid-phase extraction[J] .J China Pharm Univ(中国药科大学学报),2005,36(4):334-337. [6] LIU Y B,ZHANG M X,XUE R F.To detect organophosphorus pesticide multi-residues with GC-MS [J] .J Environ Monitor Manage Technol(环境监测管理与技术),2005,17(5):23-26. [7] ZHANG Y L,YAN Z.Progress of the technology for pesticide residue analysis in Herbal Medicines[J] .Hebei J Industirial Sci Technol(河北工业和科技杂志),2004,21(5):56-59. [8] WANG W G,LI C J,LI Y L,et al. Application of Organic Mass Spectrogram-Environment Agriculture Court of Science(有机质谱应用在环境、农业和法庭科学中的应用)[M] .Beijing:Chemical Industry Press,2005:67-153.

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