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高效液相色谱-紫外/质谱法对黄连解毒汤主要成分的定性定量测定

[Qualitative and quantitative determination of the main components of huanglianjiedu decoction by HPLC-UV/MS].

作者信息

Sun Jian, Ma Ji-sheng, Jin Jin, Wang Huai-sheng, Wen Qing-hui, Zhang Hong-gui, Zhou Qiu-li

机构信息

School of Pharmacy, Jilin University, Changchun, China.

出版信息

Yao Xue Xue Bao. 2006 Apr;41(4):380-4.

PMID:16856488
Abstract

AIM

To establish a comprehensive HPLC analytical method of Huanglianjiedu decoction.

METHODS

This study was performed by HPLC-UV/MS to identify the chemical constituents of the whole and individual herbs of the "Huanglianjiedu decoction". Zorbax Extend C18 (150 mm x 4. 6 mm ID, 5 microm) column was used; the mobile phase was composed of acetonitrile (A) and water (B, with 0.5% acetic acid) with gradient elution; the flow rate was 1.0 mL x min(-1) and the column temperature was setup at 25 degrees C. The detection wavelength was 254 nm.

RESULTS

The chromatogram of Huanglianjiedu decoction showed 21 main peaks. Peaks 1, 2, 5 and 18 were from Gardenia jasminoides Ellis, Peaks 8, 13, 14, 15, 16, 17, 19 and 21 from Scutellaria baicalensis Georgi. While 10 from Coptis chinensis Franch and 20 from Phellodendron amurense Rupr., Peaks 3, 4, 6, 9, 11 and 12 came from them together. Peak 7 presented in the chromatograms of the herbs except Gardenia jasminoides Ellis. By comparison of the retention time, the on-line UV spectra and MS spectra, 11 peaks were identified as 5 (geniposide), 9 (jatrorrhizine), 10 (coptisine), 11 (palmatine), 12 (berberine), 13 (baicalin), 15 (oroxin A), 17 (wogonoside), 19 (baicalein), 20 (obaculactone), 21 (wogonin), then eight of them were quantified by HPLC-UV.

CONCLUSION

The method could represent the characteristics of Huanglianjiedu decoction, and it could be used to evaluate the quality and quantity of Huanglianjiedu decoction. It distinguished between Coptis chinensis Franch and Phellodendron amurense Rupr. by HPLC for the first time.

摘要

目的

建立一种黄连解毒汤的综合高效液相色谱分析方法。

方法

本研究采用高效液相色谱 - 紫外/质谱联用技术对黄连解毒汤全方及单味药的化学成分进行鉴定。使用Zorbax Extend C18(150 mm×4.6 mm内径,5微米)色谱柱;流动相由乙腈(A)和水(B,含0.5%乙酸)组成,进行梯度洗脱;流速为1.0 mL·min⁻¹,柱温设定为25℃。检测波长为254 nm。

结果

黄连解毒汤色谱图显示21个主峰。峰1、2、5和18来自栀子,峰8、13、14、15、16、17、19和21来自黄芩,峰10来自黄连,峰20来自黄柏,峰3、4、6、9、11和12来自它们共同作用。峰7出现在除栀子外的各药材色谱图中。通过保留时间、在线紫外光谱和质谱光谱的比较,鉴定出11个峰分别为5(栀子苷)、9(小檗碱)、10(黄连碱)、11(巴马汀)、12(黄连素)、13(黄芩苷)、15(黄芩新素A)、17(汉黄芩苷)、19(黄芩素)、20(奥巴库内酯)、21(汉黄芩素),然后其中8种通过高效液相色谱 - 紫外进行定量分析。

结论

该方法能够体现黄连解毒汤的特征,可用于评价黄连解毒汤的质量和含量。首次通过高效液相色谱区分了黄连和黄柏。

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