目的 提出一种中成药综合质量控制的策略,并遵循该策略建立通滞苏润江制剂的HPLC分析方法。方法 该策略包括3个步骤,步骤1采用多波长进行色谱数据检测,步骤2为多元统计分析进行鉴别和定量,步骤3建立多种技术的替代对照品法。制剂使用甲醇超声提取。使用乙腈-0.1%磷酸水溶液梯度洗脱,270、350、410和440 nm 4个波长检测。并使用雷达图分析、聚类热图分析、主成分分析和夹角余弦相似度分析方法对数据进行统计。最后使用双标线性校正法、相对保留时间法和PDA光谱法进行色谱峰的定性;采用相对校正因子法进行定量。结果 同时测定没食子酸、诃子酸、秋水仙碱、番泻苷B、番泻苷A、西红花苷Ⅰ和西红花苷Ⅱ的多指标含量测定方法和评价18个特征峰的指纹图谱方法符合方法学验证的要求。数据分析表明,各企业的样品存在差异,区分各类样品的强特征峰为没食子酸、诃子酸、诃子肉、番泻叶、番泻叶和西红花苷Ⅰ。结论 该策略建立的方法全面、专属、成本较低,能有效地对通滞苏润江制剂进行质量控制。
Abstract
OBJECTIVE To propose a holistic strategy for quality control of Chinese patent medicines, and establish an HPLC analytical method for Tongzhi Surunjiang preparation according to the strategy. METHODS The strategy contained three steps.The first step was multi-wavelength chromatographic detection.The second step was multivariate analysis for identification and assay. The third step was to establish substitute reference substance method.The preparations were extracted by ultrasound with methanol, chromatography was performed on ODS column with gradient elution with acetonitrile and 0.1%phosphoric acid aqueous solution.The detection wavelengths were set at 270, 350, 410 and 440 nm.The radar chart, HCA heatmap, principal component analysis and cosine similarity were used for data analysis.At last, linear calibration using two reference substances, relative retention time method and PDA spectrum method were used for peak identification, and relative correction factor method was used for quantitative analysis. RESULTS The multi-components determination method and fingerprint analysis met the method validation requirements. Data analysis showed that there were some differences among the samples of different manufacturers. Strong characteristic peaks for classification were gallic acid, chebulinic acid, chebulea fructus, sennae folium, sennae folium and crocinⅠ.CONCLUSION The method is specific, with low cost, and could be used to accurately control the quality of Tongzhi Surunjiang preparation.
关键词
指纹图谱 /
化学计量学 /
替代对照品 /
双标线性校正法 /
中药 /
中成药 /
多波长检测 /
番泻苷B /
西红花苷Ⅰ
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Key words
fingerprint /
chemometrics /
substitute reference substance /
linear calibration using two reference substances /
traditional Chinese medicine /
Chinese patent medicine /
multiwavelength detection /
sennoside B /
crocinⅠ
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中图分类号：
R917
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参考文献
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脚注
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基金
国家自然科学基金项目资助(81303214)
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