论文部分内容阅读
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 C18(2)(4.6 mm×150 mm,5μm),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 28μg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。
Objective To identify and determine the content of piperine in four major traditional Chinese medicines in Shisuwei Black Pill. Methods TLC method was used for the qualitative identification of oriental jambalam, 荜 茇, black pepper, dried ginger and Rhododendron simsii. The content of piperine was determined by high performance liquid chromatography (HPLC). The chromatographic column was Phenomenex Luna C18 (2) (4.6 mm × 150 mm, 5 μm). The mobile phase was methanol-water (74:26) at a flow rate of 0.8 ml / min. Results TLC was detected in three batches of 15 flavors of black dehuvuccine lactone, piperine and spicy rhododendron and ginger medicinal herbs, the identification of proprietary strong TLC spots clear, negative control without (R = 0.999 8), and the average recovery rate (n = 9) was 97.76%. The results showed that piperine had a good linear relationship with other chromatographic peaks. The linear range was 0.021 056 ~ , And three batches (010624, 021008, 030323) of piperine in nine samples averaged 1.64 mg / pill. Conclusion The quality standard of Shisuowei Black Pill can be used to identify the components of five kinds of Chinese traditional medicines such as Tibetan marijuana, iguana, black pepper, dried ginger and Rhododendron simiarum, and to determine the content of piperine in the prescription.