摘要
【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 Compound Shenqu Granules （SG）. Methods With the content, fluidity and hygroscopicity of salvianolic acid B as evaluation indexes, the extraction, purification , concentration, drying and forming process of SG was studied. According to Chinese Pharmacopoeia, half medicinal materials of SG were identified by thin-layer chromatography （TLC）. With salvianolic acid B content as observation index, the optimal extraction process of SG was screened through investigating extraction methods,extraction time and solvent amount for SG. The methodological evaluation included linearity, precision, specificity, stability and accuracy of the test. HPLC method was used to determine the content of salvianofic acid B. The chromatographic analysis was carried out on Phenomenex Luna CI 8 column with octadecylsilane chemically bonded silica as loading agent. The mobile phase consisted of methanol-acetonitrile-2% water solution of formic acid （28： 10： 62）, detection wavelength was 286 nm, and external standard was applied. Results The quality of pilotplant products was good when the products were produced with the optimal forming process which was stable in laboratory. The content of salvianofic acid B of pilotplant products was the highest by the method of refluxing with 50 mL 75% hot ethanol for 30 minutes. The relevant parameters were qualified, and the accuracy and recovery rate of sample content determination met the requirement issued by Chinese Pharmacopoeia （2005）. Conclusion The optimal forming process of Compound Shenqu Granules has been established successfully. TLC analysis is set up with ginsenoside Rgl, hesperidin and harpagoside as control, which will provide a basis for the qualitative study of Compound Shenqu Granules. HPLC analysis is also established with salvianolic acid B as content determination index. The content of total saponins in the granules is determined.
出处
《广州中医药大学学报》
CAS
2011年第1期56-62,106,共8页
Journal of Guangzhou University of Traditional Chinese Medicine
基金
广东省中医药管理局基金资助项目(编号:2007167)
关键词
复方参曲颗粒剂/生产与制备
丹酚酸B/分析
总皂苷/分析
色谱法
高压液相
色谱法
薄层
COMPOUND SHENQU GRANULES/production ＆ preparation
SALVIANOLIC ACID B/analysis
TOTAL SAPONINS/analysis
CHROMATOGRAPHY, HIGH PRESSURE LIQUID
CHROMATOGRAPHY, THIN LAYER
