十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定

胡婧; 易凡力; 刘松青

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十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定

论著 | 更新时间：2026-01-09

- 十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定
- Identification of five active ingredients and content determination of piperine in Shiwuwei Heyaowan pills by TLC and HPLC
- 陆军军医大学学报 2011年33卷第6期页码：621-624
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  中图分类号： R286;R284
- 纸质出版：2011
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胡婧,易凡力,刘松青.十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定[J].陆军军医大学学报(原第三军医大学学报),2011,33(06):621-624.

　Hu Jing,Yi Fanli,Liu Songqing.Identification of five active ingredients and content determination of piperine in Shiwuwei Heyaowan pills by TLC and HPLC[J].J Amry Med Univ (J Third Mil Med Univ),2011,33(06):621-624.
胡婧,易凡力,刘松青.十五味黑药丸中4种活性成分的定性鉴别及胡椒碱的含量测定[J].陆军军医大学学报(原第三军医大学学报),2011,33(06):621-624. DOI：

　Hu Jing,Yi Fanli,Liu Songqing.Identification of five active ingredients and content determination of piperine in Shiwuwei Heyaowan pills by TLC and HPLC[J].J Amry Med Univ (J Third Mil Med Univ),2011,33(06):621-624. DOI：

摘要

目的对十五味黑药丸中4种主要中药成分进行定性鉴别并测定胡椒碱的含量。方法采用薄层色谱法（thin layer chromatography

TLC）对方中藏木香、荜茇、黑胡椒、干姜、烈香杜鹃进行定性鉴别；采用高效液相色谱法（HPLC）测定胡椒碱的含量。色谱柱：Phenomenex Luna C

(2)(4.6 mm×150 mm，5 μm)，流动相∶甲醇-水（74∶26），流速0.8 ml/min，检测波长343 nm，柱温35 ℃。结果采用TLC均能检出3批十五味黑药丸中的去氢木香内酯、胡椒碱及烈香杜鹃和干姜药材，该鉴别方法专属性强、薄层色谱斑点清晰

阴性对照无干扰；胡椒碱的HPLC色谱峰与其他色谱峰分离良好，进样量在0.021 056～0.105 28 μg范围内呈良好线性关系(r=0.999 8)，平均加样回收率(n=9)为97.76%，3个批次（010624、021008、030323）9个样品中胡椒碱的含量平均值为1.64 mg/丸。结论建立的十五味黑药丸质量标准可用于藏木香、荜茇、黑胡椒、干姜、烈香杜鹃5种中药的成分鉴别及组方中胡椒碱的含量测定。

Abstract

Objective To identify five active ingredients (Inula racemosa

Piper longum

Piper nigrum

Zingiber officinale and Rhododendron anthopogonoides) and determine the content of piperine in traditional Tibetan medicine pills—Shiwuwei Heiyaowan. Methods Three batches of Shiwuwei Heiyaowan pills were dissolved in ethyl ether or absolute ethyl alcohol as the sample solutions. Thin layer chromatography (TLC) was utilized to identify Inula racemosa

Piper longum

Piper nigrum

Zingiber officinale and Rhododendron anthopogonoides in

Shiwuwei Heiyaowan pills. High performance liquid chromatography (HPLC) was employed to determine the content of piperine. In HPLC

the chromatographic column is Phenomenex Luna C

(2) (4.6 mm×150 mm

5 μm); the mobile phase is methanol-water (74∶26); the flow rate is 0.8 ml/min; the detection wavelength is 343 nm; the column temperature is 35 ℃. Results In TLC

dehydrocostunolide lactone (the characteristic compound of Inula racemosa)

piperine (the characteristic compound of Piper longum and Piper nigrum)

Rhododendron anthopogonoides and Zingiber officinale were identified in all batches of Shiwuwei Heiyaowan pills. The identification method was highly specific with clear TLC spots. The negative control did not impose any disturbance. In HPLC

the chromatographic peak of piperine was well isolated from other peaks. There was a good linear relationship between the sample size and the peak area of piperine in a range of 0.021 056-0.105 28 μg (r=0.999 8). The average recovery of piperine was 97.76% (n=9). The average piperine content of nine samples (three from each batch) was 1.64 mg/pill. Conclusion The constructed quality standards can be utilized to identify Inula racemosa

Piper longum

Piper nigrum

Zingiber officinale and Rhododendron anthopogonoides

as well as determine the content of piperine in Shiwuwei Heiyaowan pills.

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