快速液相色谱-串联质谱法测定果实类药材中的黄曲霉毒素

栗建明 李纯 顾利红 江英桥

中国药学杂志 ›› 2012, Vol. 47 ›› Issue (1) : 65-68.

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中国药学杂志 ›› 2012, Vol. 47 ›› Issue (1) : 65-68.
论著

快速液相色谱-串联质谱法测定果实类药材中的黄曲霉毒素

  • 栗建明,李纯,顾利红,江英桥
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Determination of Aflatoxins in Fruit Traditional Chinese Medicines by Rapid-Resolution Liquid Chromatography Tandem Mass Spectrometry

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摘要

目的 建立中药材中4种黄曲霉毒素测定的快速液相色谱-串联质谱方法。方法 样品经体积分数70%甲醇提取、免疫亲和柱净化,岛津Shim-pack XR-ODS色谱柱,用甲醇-乙腈(1∶1)和水为流动相,梯度洗脱,ESI扫描,多反应监测(MRM)。结果 黄曲霉毒素B1在0.102 1~10.21 ng·mL内、黄曲霉毒素B2在0.061 2~7.65 ng·mL内、黄曲霉毒素G1在0.193~9.65 ng·mL内、黄曲霉毒素G2在0.121~7.55 ng·mL内,线性关系均良好,r>0.999 8;4种黄曲霉毒素回收率在77.0%~102.4%之间。结论 本方法准确可靠,适合中药材中4种黄曲霉毒素含量的测定。

Abstract

OBJECTIVE To develope a method for determination of four aflatoxins (B1, B2, G1, G2) in fruit traditional Chinese medicines by rapid-resolution liquid chromatography coupled with electrospray ionization triple quadrupole tandem mass spectrometry. METHODS After being extracted with 70% methanol and purified by immunoaffinity columns, the four aflatoxins were separated on a Shim-pack XR-ODS column using gradient elution with the mobile phase of CH3CN-CH3OH-H2O mixtures monitored under MRM mode in ESI positive scan. RESULTS There was a good linear relationship over the range of 0.102 1-10.21 ng·mL for AFB1, 0.061 2-7.65 ng·mL for AFB2, 0.193-9.65 ng·mL for AFG1, 0.121-7.55 ng·mL for AFG2 (r>0.999 8), respectively. The average recoveries ranged from 77.0%-102.4%. CONCLUSION This method provides a simple and feasible way to determine aflatoxins.

关键词

快速液相色谱-串联质谱 / 黄曲霉毒素 / 果实类 / 中药材

Key words

RRLC-MS/MS / aflatoxins / fruit / traditional Chinese medicine

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栗建明 李纯 顾利红 江英桥. 快速液相色谱-串联质谱法测定果实类药材中的黄曲霉毒素[J]. 中国药学杂志, 2012, 47(1): 65-68
Determination of Aflatoxins in Fruit Traditional Chinese Medicines by Rapid-Resolution Liquid Chromatography Tandem Mass Spectrometry[J]. Chinese Pharmaceutical Journal, 2012, 47(1): 65-68

参考文献


[1] GB/T5009. 22-2006(中华人民共和国国家标准) [S]. 2007:1-7.
[2] Ch. P (2010) Vol Ⅱ(中国药典2010年版. 一部)[S]. 2010: Appendix 60-61.
[3] GB/T 17480-2008. Determination of aflatoxin B1 in feeding stuffs-Enzyme-linked immunosorbent assay[S]. 2009:1-3.
[4] VENTURA M, GOMEZ A, ANAYA I, et al. Determination of aflatoxins B1, G1, B2 and G2 in medicinal herbs by liquid chromatography-tandem mass spectrometry[J]. J Chromatogr A, 2004, 1048 (1):25-29.
[5] REN Y P, YU Z, SHAO S L, et al. Simultaneous determination of multi-component mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography tandem mass spectrometry[J]. J Chromatogr A, 2007,1143(1-2):48-64.

基金

国家科技重大专项-重大新药创新课题(中药中有害残留检测技术标准平台课题编号 2009ZX09308-006)资助项目
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