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【目的】研究复方参曲颗粒剂的制备和质量标准。【方法】以丹酚酸B的含量、流动性和引湿性等为指标,考察复方参曲颗粒剂的提取、纯化、浓缩、干燥、成型等工艺。以处方半数药材为研究对象,依据中国药典进行薄层鉴别;以丹酚酸B的含量为指标,通过对成品的提取方法、提取时间、溶剂用量3个方面进行选择,建立成品最佳提取方法;方法学考察包括线性、精密度、专属性、稳定性、准确度等内容。采用高效液相色谱(HPLC)法测定丹酚酸B的含量,以十八烷基硅烷键合硅胶为填充剂,甲醇—乙腈—体积分数2%甲酸水(体积比为28∶10∶62)为流动相,检测波长为286 nm,按外标法定量。【结果】将小试最佳成型工艺进行3批放大中试生产,结果证明产品工艺稳定,符合质量标准规定;成品提取用体积分数75%甲醇50 mL,加热回流30 min所得的丹酚酸B含量最高,各项实验结果均符合相应参数的要求,说明采用的方法满足相应的检测要求。样品含量测定方法准确度、回收率均符合中国药典Ⅰ部(2005版)。该方法灵敏度高、专属性强。【结论】本实验筛选出了复方参曲颗粒剂最佳成型工艺。建立了以人参皂苷Rg1、橙皮苷、哈巴俄苷为对照品的薄层鉴别方法,为复方参曲颗粒剂的定性研究提供了依据;建立了以丹酚酸B为含量测定指标的HPLC法;建立了成品总皂苷含量测定方法。
【Objective】 To study the preparation and quality standard of Fufang Shenqu Granule. 【Method】 The contents of salvianolic acid B, fluidity and hygroscopicity were taken as indexes to investigate the extraction, purification, concentration, drying and forming of Fufang Shenqu Granule. Taking half of the prescriptions as the research object and thin layer identification according to the Chinese Pharmacopoeia. Using the content of salvianolic acid B as an index, the best extraction method of finished products was established through three aspects: extraction method, extraction time and solvent dosage Methodological studies include linearity, precision, specificity, stability, accuracy and so on. The content of salvianolic acid B was determined by high performance liquid chromatography (HPLC). The octadecylsilane bonded silica gel was used as the filler, methanol - acetonitrile - 2% formic acid with a volume fraction of 28:10:62 As mobile phase, detection wavelength of 286 nm, according to external standard method. 【Result】 The results showed that the product process was stable and accorded with the quality standard. The final product was extracted with 50 mL of 75% methanol by volume and heated at reflux for 30 min to obtain salvianolic acid B The highest content, the experimental results are in line with the requirements of the corresponding parameters, indicating the method used to meet the appropriate testing requirements. The accuracy of the method for the determination of the sample content, the recovery rate are in line with the Chinese Pharmacopoeia Ⅰ (2005 Edition). The method has high sensitivity and specificity. 【Conclusion】 This experiment screened out the best forming process of Compound Shenqu Granule. The TLC identification method of ginsenoside Rg1, hesperidin and harpagoside was established, which provided the basis for the qualitative study of Compound Shenqu Granule. The HPLC method was established to determine the content of salvianolic acid B The method of determination of total saponin content was established.