济川煎中4种指标成分同时测定及其物质基准工艺研究

Study on simultaneous determination of four index components in Jichuan Decoction and it's material standard technology

关键词:  经典名方  济川煎  物质基准  质量控制  制备工艺

Key words:  classical prescription  Jichuan Decoction  material standard  quality control  preparation process

摘要:

[目的] 采用高效液相色谱(HPLC)法建立经典名方济川煎指纹图谱,同时测定柚皮苷、新橙皮苷、β-蜕皮甾酮、松果菊苷4种指标成分的含量及建立其物质基准制备工艺,以全面评价和有效控制济川煎的质量。[方法] 采用Agilent ZORBAX SB-C₁₈(4.6 mm×250 mm,3.5 μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,柱温30℃,流速为1.0 mL/min进行梯度洗脱;并对其物质基准制备工艺进行考察,优选最佳工艺制备方法。[结果] 建立了济川煎指纹图谱共有模式,12批样品的指纹图谱与共有模式相比其相似度良好,确定了14个共有峰,并对其中6个共有峰进行了指认归属;柚皮苷、新橙皮苷、β-蜕皮甾酮、松果菊苷含量分别在3.46~5.87、3.35~5.36、0.19~0.23、0.72~7.02 mg/g,方法学考察结果显示各项指标均符合含量测定要求。物质基准制备工艺为:精密称取处方量药材,加超纯水300 mL,浸泡45 min,武火沸后文火加盖煎煮至130~140 mL,3层纱布趁热过滤,绞渣,放冷,滤液70℃减压浓缩后冷冻干燥,即得干膏粉。[结论] 所建立的济川煎HPLC指纹图谱共有模式特征性强,多指标成分的含量测定及物质基准制备工艺的研究为济川煎物质基准的深入研究提供数据参考。

Abstract:

[Objective] To establish a method for the fingerprint and quantitative analysis of four components (naringin,neohesperidin,β-ecdysterone,and echinacoside) in Jichuan Decoction by HPLC. At the same time,the material reference technology research method was investigated to provide reference for scientific evaluation and quality control.[Methods] The HPLC analysis was performed on an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm,3.5 μm) in a gradient elution program with acetonitrile-0.1% phosphoric acid solution as the mobile phase. The column temperature was set at 30℃,andthe flow rate was1.0 mL/min. The preparation process method of Jichuan Decoction was investigated to selectthe best process research method.[Results] A common pattern of HPLC fingerprint of Jichuan Decoction was established. Compared with the common pattern,the similarities of 12 batches of samples were above 0.950 with 14 common peaks,and six of which were identified and assigned. The contents of naringin,neohesperidin,β-ecdysterone,and echinacoside all within the range of 3.46 to 5.87 mg/g,3.35 to 5.36 mg/g,0.19 to 0.23 mg/g and 0.72 to 7.02 mg/g,respectively. The results of methodology study also showed that all indexes meet the requirements of content determination. The material reference technology research method wasas follows:accurately weighed the prescription amount of medicinal materials,added 300 mL of ultra-pure water,soaked for 45 min,boiled after boiling,covered and decocted to 130 to 140 mL,filtered with three layers of gauze while hot,twisted the slag,and let cool,The filtrate was concentrated under reduced pressure at 70℃ and freeze-dried to obtain the Jichuan Decoction material reference dry paste powder.[Conclusion] The established common pattern of HPLC fingerprint of Jichuan Decoction has good characteristics. Combined with the content determination of multiple index components,the material reference technology research methods are also conductive to promote the quality control of the preparation of Jichuan Decoction.