经典名方苏葶丸的质量控制方法研究

Research on the quality control method of classical Suting Pills

关键词:  苏葶丸  质量控制  薄层色谱  指纹图谱  含量测定

Key words:  Suting Pill  quality control  TLC  fingerprint spectrum  content determination

摘要:

[目的] 建立经典名方苏葶丸的质量控制方法。[方法] 采用薄层色谱法（TLC）定性鉴别苏葶丸中的炒紫苏子和炒葶苈子；采用高效液相色谱法（HPLC）进行定量分析，并建立指纹图谱。色谱柱为InfinttyLab Poroshell 120 EC-C₁₈（4.6 mm×150 mm，4 μm），进样量为8 μL，柱温30 ℃，流速为0.8 mL/min，以0.1%磷酸水溶液（A）-乙腈（B）为流动相梯度洗脱（0~6 min，7%~9%B；6~30 min，9%~43%B；30~32 min，43%~90%B；32~40 min，90%B）。指纹图谱及槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷含量测定波长为254 nm，迷迭香酸为320 nm。采集10批苏葶丸指纹图谱，利用“中药色谱指纹图谱相似度评价系统”（2012年版）进行相似度评价，并使用HPLC法同时测定2种指标成分含量。[结果] 薄层色谱分离效果良好，特征斑点显示清晰，且阴性对照无干扰。10批苏葶丸指纹图谱相似度均大于0.9，共标定7个共有峰。槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷和迷迭香酸的平均加样回收率分别为99.90%、96.06%，RSD均小于3%，各成分在一定进样范围内呈现良好的线性关系。10批苏葶丸中槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷和迷迭香酸的质量分数范围分别为0.081~0.459、1.228~1.618 mg/g。[结论] 该方法简便、稳定、准确可靠，可用于苏葶丸的质量控制，同时为苏葶丸的相关制剂开发奠定基础。

Abstract:

[Objective] To establish the quality control method of classical Suting Pills. [Method] TLC was used to characterize the identification of fried Perilla frutescens seed and stir-fried Descurainiae Semen in Suting Pills. High performance liquid chromatography（HPLC） was used for quantitative analysis and fingerprinting. The column was InfinttyLab Poroshell 120 EC-C₁₈ column（4.6×150 mm，4 μm），with an injection volume of 8 μL，a column temperature of 30 ℃，a flow rate of 0.8 mL/min，and a gradient elution with 0.1% phosphoric acid aqueous solution（A）-acetonitrile（B） as the mobile phase（0~6 min，7%~9%B；6~30 min，9%~43%B；30~32 min，43%~90%B；32~40 min，90%B）. The fingerprint and the detection wavelength of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside were 254 nm，and rosmarinic acid was 320 nm. The fingerprints of 10 batches of Sufa Pills were collected and evaluated for similarity using the “Chinese Medicine Chromatographic Fingerprint Evaluation System”（2012 Eidition），and the contents of the two index components were determined simultaneously using the HPLC method. [Results] he results of TLC separation were good，the characteristic spots were clearly displayed，and there was no interference in the negative control. The similarity of the fingerprints of 10 batches of Sulphur scape pills was greater than 0.9，and a total of 7 common peaks were identified. The average spiked recoveries of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside and rosmarinic acid were 99.90% and 96.06%，respectively，and the RSD was less than 3%，and the components showed a good linear relationship within a certain injection range. The mass fractions of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside and rosmarinic acid in 10 batches of Suting Pills ranged from 0.081~0.459 and 1.228~1.618 mg/g，respectively. [Conclusion] This method is simple，stable，accurate and reliable，and can be used for the quality control of Suting Pills，as well as laying the foundation for the development of related formulations of Suting Pills.