气相色谱-质谱联用法同时测定中药材中53种农药残留方法

苗水 陆继伟 郏征伟 毛秀红 李雯婷 王柯 季申

中国药学杂志 ›› 2010, Vol. 45 ›› Issue (16) : 1263-1269.

PDF(1172 KB)
PDF(1172 KB)
中国药学杂志 ›› 2010, Vol. 45 ›› Issue (16) : 1263-1269.
论 著

气相色谱-质谱联用法同时测定中药材中53种农药残留方法

  • 苗水,陆继伟,郏征伟,毛秀红,李雯婷,王柯,季申*
作者信息 +

Simultaneous Determination of 53 Pesticide Residues in Traditional Chinese Herbal Medicines by GC/MS

  • MIAO Shui, LU Ji-wei, JIA Zheng-wei,MAO Xiu-hong,LI Wen-ting,WANG Ke, JI Shen*
Author information +
文章历史 +

摘要

目的 采用气相色谱-质谱法研究中药材中农药多残留的测定方法方法 选用代表性的白果、人参、肉桂、红花、银杏叶、广藿香等中药材样品进行研究,样品经乙腈匀浆萃取,依次经碳十八、石墨化碳与氨丙基串联固相萃取小柱净化后,采用气相色谱-质谱同时定性、定量测定。结果 在6种中药材样品基质、3水平添加条件下,53种农药的回收率大多在70.0%~120.0%,相对标准偏差小于20%,检测限大多低于0.01 mg·kg-1,符合农药多残留检测的要求。结论 本法净化效果好,灵敏度高,重现性好,可用于中药材样品中农药多残留的日常检测。

Abstract

OBJECTIVE To develop the multi-residues methods for traditional Chinese herbal medicines(TCHMs) by GC-MS. METHODS 6 representative samples(Semen Ginkgo,Radix Ginseng,Cortex Cinnamomi,Flos Carthami, Folium Ginkgo,and Herba Pogostemonis)were selected as experimental materials. The selected samples were extracted by acetonitrile, and then cleaned by C18 and Envi-carb/PSA solid phase extraction (SPE) cartridges. The residue detection was carried out by GC-MS. RESULTS The analytical performance was demonstrated by the analysis of 6 TCHMs samples' extracts, fortified at three levels for each pesticide. In general, the recoveries ranged from 70% to 120% and relative standard deviations (RSDs) were all less than 20%. The limits of detection (LODs) for most of the selected pesticides were below 0.01 mg·kg-1. CONCLUSION The method shows high sensitivity,good repeatability and satisfactory cleaning-up excellence, which could be applied to the pesticide residue detection for the TCHMs.

关键词

中药材 / 农药残留 / 固相萃取 / 气相色谱-质谱法

Key words

traditional Chinese herbal medicines(TCHMs) / pesticides residues / solid phase extraction / gas chromatography-mass spectrometry

引用本文

导出引用
苗水 陆继伟 郏征伟 毛秀红 李雯婷 王柯 季申. 气相色谱-质谱联用法同时测定中药材中53种农药残留方法[J]. 中国药学杂志, 2010, 45(16): 1263-1269
MIO Shui;LU Ji-wei;JI Zheng-wei;MO Xiu-hong;LI Wen-ting;WNG Ke;JI Shen. Simultaneous Determination of 53 Pesticide Residues in Traditional Chinese Herbal Medicines by GC/MS[J]. Chinese Pharmaceutical Journal, 2010, 45(16): 1263-1269

参考文献


[1] Ch .P(2000)(中国药典2000年版.一部) [S]. 2000:appendix 60.
[2] Ch .P(2005)(中国药典2005年版.一部) [S].2005:appendix 52-54.
[3] GB/T 19648-2006. Method for determination of 500 pesticides and related chemicals residues in fruits and vegetables by GC-MS method [S]. 2006:1-68.
[4] GB/T 19649-2006.Method for determination of 475 pesticides and related chemicals residues in grains by GC-MS method [S]. 2006:1-68.
[5] GB/T 19650-2006.Method for determination of 478 pesticides and related chemicals residues in animal muscles by GC-MS method [S]. 2006:1-68.
[6] GB/T 19426-2006.Method for the determination of 497 pesticides and related chemicals residues in honey, fruit juice and wine by GC-MS method [S]. 2006:1-68.
[7] GB/T 20769-2006.Method for determination of 405 pesticides and related chemicals residues in fruits and vegetables by LC-MS-MS method [S]. 2006:1-70.
[8] GB/T 20770-2006.Method for determination of 372 pesticides and related chemicals residues in grains by LC-MS-MS method [S].2006:1-64.
[9] GB/T 20771-2006.Method for the determination of 420 pesticides and related chemicals residues in honey, fruit juice and wine by LC-MS-MS method [S].2006:1-71.
[10] GB/T 20772-2006. Method for determination of 380 pesticides and related chemicals residues in animal muscles LC-MS-MS method [S].2006:1-65.
[11] FILLION J, SAUVE F. Multiresidue method for the determination of residues of 251 pesticides in fruits and vegetables by gas chromatography/mass spectrometry and liquid chromatography with fluorescence detection[J]. J AOAC Int, 2000, 83(3): 698-713.
[12] CAO Y Z, PANG G F, ZHANG J J,et al.Determination of Residues of 446 Pesticides in Fruits and Vegetables by Three-Cartridge Solid-Phase Extraction-Gas Chromatography-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry[J]. J AOAC Int(国际官方分析化学师协会会志), 2006, 89(3): 740-771.
[13] LEHOTAY S J, KATERINA M, YUN S J. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes[J]. J AOAC Int(国际官方分析化学师协会会志), 2005, 88(3): 630-638.
[14] MICHELANGELO A, KATERINA M, LEHOTAY S J. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J]. J Chromatogr A(色谱), 2003, 1015(1): 163-184.
PDF(1172 KB)

Accesses

Citation

Detail

段落导航
相关文章

/