防风煮散饮片工艺开发与质量控制研究

Development and Quality Control Study on the Processing of Saposhnikoviae Radix Decoction Granules

中文关键词:防风煮散饮片  工艺开发  质量控制  DNA 条形码  含量测定  稳定性试验

keywords:Saposhnikoviae Radix decoction granules  Process development  Quality control  DNA barcoding  Content determination  Stability test

中文摘要:摘要 目的：本研究旨在开发防风煮散饮片的制备工艺并建立其质量控制方法，以实现对防风煮散饮片的标准化制备。方法：通过对防风药材进行净制、切制等预处理，以形态、粒度分布、指标成分（升麻素苷、5-O - 甲基维斯阿米醇苷）煎出率等为评价指标，筛选最佳制备工艺，建立融合 DNA 条形码技术（ITS2 序列）与薄层色谱的真伪鉴别体系，基于高效液相色谱测定升麻素苷与5-O-甲基维斯阿米醇苷总含量；通过加速（40℃/75% RH）与长期（30℃/60% RH）稳定性试验考察 6个月质量变化。结果：最优饮片炮制工艺得率86.2%，煮散饮片采用5.0 mm孔径筛网的破碎机破碎，用0.8 mm及8.0 mm筛网整粒，其平均收率为83.1%，与传统饮片对比，不同时间溶出中出膏率、醇溶率、成分转移率不存在显著性差异（P>0.05），经多批次验证，出膏率、醇溶率、浸出物、指标成分含量、及成分转移率均不存在显著性差异（P>0.05）。稳定性试验中指标成分RD＜10.0%。结论：防风煮散饮片制备工艺稳定可控，质量控制体系具专属性与灵敏度，以出膏率、醇溶率、指标成分含量与转移率为评价指标，以煮散饮片成分平均转移率略高于传统饮片，且稳定性较好，工业化适配性较优，为中药饮片智能化调配及标准化生产提供了可复制的技术示范。

Abstract:ABSTRACT Objective: This study aimed to develop a preparation process and establish a quality control method for Saposhnikoviae Radix decoction granules to achieve standardized production. Methods: Raw materials were pre-treated (cleaning, cutting). Morphology, particle size distribution, and the decoction yield of marker compounds (prim-O-glucosylcimifugin and 4’-O-β-glucosyl-5-O-methylvisamminol) were used as evaluation indexes to optimize the preparation process. An identification system integrating DNA barcoding (ITS2 sequence) and thin-layer chromatography (TLC) was established for authenticity verification. The total content of prim-O-glucosylcimifugin and 4’-O-β-glucosyl-5-O-methylvisamminol was determined using high-performance liquid chromatography (HPLC). Quality changes over 6 months were assessed through accelerated (40°C at 75% relative humidity (RH)) and long-term (30°C at 60% RH) stability studies. Results: The optimized primary decoction piece processing yield was 86.2%. decoction granules were prepared by crushing material through a 5.0 mm screen, followed by sieving through 0.8 mm and 8.0 mm screens, yielding an average granulation rate of 83.1%. Compared with traditional decoction pieces, there were no significant differences (P>0.05) in extract yield, alcohol-soluble yield, or compound transfer rate at different time points during dissolution. Multi-batch verification confirmed no significant differences in extract yield, alcohol-soluble yield, extractives (P=0.07), marker compound content, or compound transfer rate. The relative deviations (RD) of marker compounds were less than 10.0% in stability tests. Conclusion: The preparation process for Saposhnikoviae Radix decoction granules is stable and controllable. The established quality control system is specific and sensitive. Based on evaluation indexes such as extract yield, alcohol-soluble yield, marker compound content, and transfer rate, the decoction granules demonstrated slightly higher average marker compound transfer compared to traditional decoction pieces, good stability, and superior adaptability to industrial production. This study provides a replicable model for intelligent dispensing and standardized production of Chinese herbal decoction pieces.