小柴胡颗粒制剂-药材谱峰匹配指纹图谱研究

目的 建立小柴胡颗粒制剂的多波长指纹图谱并进行药材-制剂谱峰匹配研究，进一步验证单一波长下指纹图谱质量评价的局限性。方法 采用RP-HPLC法对3个厂家各3个批次及实验室自制3批小柴胡颗粒（共12批样品）进行多波长指纹图谱相似性评价，并与相同色谱条件下的实验室自制小柴胡颗粒时所用的原药材指纹图谱进行谱峰匹配；RP-HPLC法测定不同来源的小柴胡颗粒中的指标成分的量。结果 在210、254、280、323 nm 4个波长下，同一药厂3个批次小柴胡颗粒之间及实验室自制的3批制剂之间的指纹图谱相似度差别较小，不同厂家的制剂之间，仅A厂制剂与实验室自制的3批制剂在4个波长下相似度均在0.9以上，其余二药厂除280 nm波长相似度在0.9以上外，在210、254、323 nm的相似度均小于0.9。在210、254、280、323 nm 4个波长，柴胡、甘草、党参和黄芩与小柴胡颗粒模式指纹图谱分别有5、5、2、18个色谱峰匹配；不同来源的小柴胡颗粒制剂中甘草酸和黄芩苷的量差异较大。在制剂中未能检测到柴胡皂苷a和d、阿魏酸、苍术内酯III、党参炔苷。结论 仅以280 nm波长指纹图谱相似度评价小柴胡颗粒制剂的质量存在很大的局限性。由于制剂过程及工艺的影响，部分药材的指标成分并未在制剂中测得；多波长相似度评价结合制剂用药材与制剂指纹图谱谱峰匹配及活性组分的定量测定相结合的方法，可为较全面评价中药制剂质量提供参考。

Fingerprint study on Xiaochaihu Granules-medicinal materials based on peak pattern matching

Objective To establish Xiaochaihu Granules multi-wavelength fingerprints and conduct Bupleuri Radix-preparations peaks matching studies for further limitation validation of a single wavelength fingerprint quality evaluation. Methods RP-HPLC was adopted to estimate the similarity on three batches of Xiaochaihu Granules from three manufacturers and three batches of Xiaochaihu Granules by laboratory-made (total 12 batches), and make peaks match raw herbs under the same conditions; the contents of indicator ingredients in different batches of Xiaochaihu Granules were determined by RP-HPLC method. Results There was few differences of the fingerprint similarities among the three batches of Xiaochaihu Granules both from the same manufacture and laboratory-made at the wavelength of 210, 254, 280, and 323 nm. Among the fingerprints of Xiaochaihu Granules from different manufactures, the similarities of Xiaochaihu Granules only from manufacture A and of the three batches of Xiaochaihu Granules from the laboratory-made were over 0.9 under the four wavelengths. The similarities from the other two manufacturers were over 0.9 except 280 nm, but less than 0.9 at the wavelength of 210, 254, and 323 nm. At 210, 254, 280, and 323 nm wavelengths, peak pattern matching showed that Xiaochaihu Granules had 5, 5, 2, and 18 matching peaks with Bupleuri Radix, Glycyrrhizae Radix et Rhizoma, Codonopsis Radix, and Scutellariae Radix, respectively. The contents of glycyrrhizic acid and baicalin in Xiaochaihu Granules from different manufactures were significantly different. Saikosaponins a and d, ferulic acid, atractylenoide III, and lobetyolin were not detected in the formulations. Conclusion There are great limitations to estimate quality of Xiaochaihu Granules with the fingerprint similarity at 280 nm. Multi-wavelength similarity evaluation combined with the peak matching of fingerprint for medicinal materials and preparations and quantitative determination of active components could provide a reference for the comprehensive quality evaluation of preparations for Chinese materia medica.