【作者】 张海茹；

【导师】 丁平田；

【作者基本信息】 沈阳药科大学 ， 药物制剂， 2007， 硕士

【摘要】 骨碎补的有效部位是总黄酮。本研究以紫外分光光度法测定了骨碎补提取物中总黄酮的含量，结果总黄酮的含量均大于50％。本研究建立了反相高效液相色谱法同时测定骨碎补总黄酮中新北美圣草苷和柚皮苷含量的方法。方法学考察表明，该方法准确、方便、重现性好。本文对骨碎补药材的提取工艺进行了研究。以总黄酮含量为评价指标进行正交试验，确定了最优提取工艺为：10倍量的60％乙醇为提取溶剂，提取3次，每次90 min。本文研究了用大孔吸附树脂对总黄酮进行纯化的工艺，通过不同种类大孔吸附树脂静态饱和吸附和解吸以及动态吸附和解吸的考察，以总黄酮为评价指标，对吸附时间、树脂种类、样品上样量、洗脱溶剂浓度和大孔树脂的稳定性进行了系统的研究。结果优选用D-101大孔吸附树脂进行纯化，洗脱溶剂为70％乙醇。骨碎补总黄酮经精制后，符合中药注射剂的技术要求。本文采用冷冻干燥技术制备注射用骨碎补总黄酮。经试验考察得到最佳处方和制备工艺，选用100 g·L^-1的甘露醇作为冻干粉针剂的赋形剂。冻干产品外形饱满，成型性、复溶性良好。对注射用骨碎补总黄酮进行了影响因素试验，结果表明样品应在遮光、阴凉处保存。以柚皮苷为参照物，使用ODS色谱柱，以甲醇-水（磷酸调pH 3.0）为流动相进行梯度洗脱，紫外法检测，建立了体现骨碎补总黄酮及其制剂化学成分的HPLC指纹图谱。方法学考察表明，该分析方法的重现性良好。采用“指纹图谱相似度评价系统”软件进行分析，10批骨碎补总黄酮及其冻干粉针剂的相似度均在0.90以上。骨碎补总黄酮与其冻干粉针剂的指纹图谱具有很好的相关性。该分析方法的建立为控制注射剂的制备工艺及产品的稳定性提供了保证。更多还原

【Abstract】 The total flavonoid is the main effective parts of Drynariae fortunei（Kunze）J.Sm.. The flavonoids in extract of Drynariae fortunei（Kunze）J.Sm. was determined by UV spectrophotometry and its content is more than 50％. An RP-HPLC method was developed for simultaneous determination of neoeriocitrin and naringin in total flavonoids of Drynaria fortunei（Kunze） J.Sm.. The method of determination is simple and accurate with good reproducibility.The optimal extraction process of Drynariae fortunei（Kunze）J.Sm, was studied by orthogonal design with the content of total flavonoid as quality control criteria. The optimal condition was 60％ethanol consumed 10 times of the amount of raw material, triplicate extraction and 90 minutes for each time. This paper studied the purifying of total flavonoid with microporous resin. Different types of microporous resin, absorption time, the sample quantity, concentration of ethanol eluting macroporous resin and utilization time of chromatogram column were studied with the content of total flavonoid as quality control criteria. D-101 macroporous resin was used to purify the extract and the 70％ethanol as the eluting solvent. The refined total flavonoids of Drynariae fortunei（Kunze）J.Sm. confirmed the standard of Chinese herbal injection.Total flavonoids of Drynariae fortunei（Kunze）J.Sm. for injection was prepared by Freeze-drying techniques. The formulation and preparation technologies were optimized, and 100 g·L^-1 mannitol was used as excipient. The freeze-dried products were examined by the critertion of appearance, redissolution. The results of stress testing indicated that the preparation should be preserved in the cool and protected from light.With naringin as reference substance, an HPLC-Fingerprints that could indicate substances existing in total flavonoids of Drynaria fortunei（Kunze）J.Sm. and its injection was established with an ODS column, ultraviolet detection and CH₃OH—water（pH at 3.0 by phosphoric acid）as mobile phase for gradient elution. The method showed a satisfactory reproducibility. Analyzed by Computer Aided Similarity Evaluation System, the HPLC- Fingerprints similarities of total flavonoids of Drynaria fortunei（Kunze）J.Sm. and its injection of 10 batches were over 0.90. There was a good correaltionship among total flavonoids of Drynaria fortunei（Kunze）J.Sm. and its injection. The method offers guarantee for the stability of the preparation techniques and final products of total flavonoids of Drynaria fortunei（Kunze）J.Sm. for injection.更多还原