论文部分内容阅读
针对中药复方制剂六味地黄丸的质量控制提出了一种多指标全药材整体分析新策略。从组成六味地黄丸的每一味药材中选取1~2个药效成分,即选取熟地黄中的毛蕊花糖苷、山茱萸中的莫诺苷和马钱苷、牡丹皮中的丹皮酚和芍药苷、山药中的尿囊素、茯苓中的茯苓酸、泽泻中的23-乙酰泽泻醇B作为六味地黄丸的质量控制指标成分,采用快速、简便、高效的超声细胞粉碎提取(UCGE)法对这8个指标成分进行同步提取。用响应曲面分析中的Box-Behnken模式对UCGE提取过程中对提取效率影响较大的料液比、提取时间和提取温度等参数进行了优化。得到最优的提取条件:料液比1∶45(g/mL)、提取时间40 min、提取温度20℃。进一步利用超高效液相色谱-二极管阵列检测(UPLC-PAD)技术实现多指标成分在同一根色谱柱上的同步分离和检测,从而建立六味地黄丸的多指标全药材整体色谱。采用HSS T3色谱柱(50 mm×2.1 mm,1.8μm),以乙腈-水为流动相进行梯度洗脱,基于指标成分的紫外光谱特征选择5个检测波长同时检测,并进行了线性关系、检出限、定量限、精密度、稳定性、重复性、准确性等方法学验证。该研究为六味地黄丸质量标准的建立提供了依据,同时也为中药复方制剂提供了一种质量控制新模式和新理念。
Aiming at the quality control of Liuweidihuangwan, a compound traditional Chinese medicine preparation, a new strategy of overall analysis of multi-index whole medicinal materials was proposed. From the composition of Liu Wei Di Huang Wan herbs for each flavor to choose 1 or 2 ingredients, that is, selected Rehmannia glutinosa in Rehmannia, cornus and loganin in dogwood, paeonol Paeoniflorin Paeoniflorin, Allantoin in yam, Poria cocos in Poria cocos, 23-acetyl alisol B in Alisma orientalis were used as quality control index components of Liuweidihuangwan, and the method of rapid, simple and efficient ultrasonic cell disruption extraction (UCGE) The eight index components were extracted simultaneously. The Box-Behnken model in response surface analysis was used to optimize the parameters such as solid-to-liquid ratio, extraction time and extraction temperature that greatly influenced the extraction efficiency during UCGE extraction. The optimal extraction conditions were as follows: solid-liquid ratio 1:45 (g / mL), extraction time 40 min, extraction temperature 20 ℃. Furthermore, UPLC-PAD was used to realize the simultaneous separation and detection of multi-index components on the same column, so as to establish the multi-index whole medicine whole chromatogram of Liuweidihuangwan. HSE T3 column (50 mm × 2.1 mm, 1.8 μm) was used for gradient elution with acetonitrile-water as the mobile phase. Based on the UV spectral characteristics of the indicator components, five detection wavelengths were selected for simultaneous detection and the linear relationship was detected Out of limits, quantitative limits, precision, stability, repeatability, accuracy and other methodological verification. The study provided the basis for establishing the quality standard of Liuwei Dihuang Pill and provided a new quality control mode and new concept for the preparation of Chinese traditional medicine.