目的以注射用芪红脉通微滤后药液为研究对象,考察4种不同材质的中空纤维超滤膜对注射用芪红脉通药液体系的适用性。方法分别选取截留相对分子质量为100 000的聚砜、聚醚砜、聚丙烯、混纺复合4种材质的超滤膜进行超滤,测定不同膜材质超滤过程的膜通量,指标成分黄芪总皂苷、黄芪甲苷、羟基红花黄色素A（hydroxy safflower yellowA,HSYA）透过率,固含物减少率,蛋白质减少率,有关物质及热原检查,筛选适宜本产品的超滤膜。结果相同截留相对分子质量的4种不同材质超滤膜对同一药液体系的适用性存在差异:聚丙烯、聚醚砜和混纺复合材质的膜纯水通量恢复率均较高,而聚砜材质的膜通量和膜纯水通量恢复率较低;聚丙烯与聚醚砜材质的指标成分透过率较高,聚砜与混纺复合材质的固含物与蛋白质去除率较高;对于本产品,截留相对分子质量为100 000超滤膜可有效去除热原。结论聚丙烯-100000超滤膜既能有效去除固含物与高分子物质,又能保留有效成分,适用于注射用芪红脉通的精制。

Objective To optimize the impurity removal technology before ultrafiltration,taking Qihong Maitong Injection(QMI) as the research object.Methods The removal of impurities and related substances by the combined process of refrigeration,centrifugation,and activated carbon adsorption was investigated.Taking the contents of total saponins of astragalus,astragaloside,and hydroxy safflower yellow pigment A,solids reduction efficiency,protein concentration,and related substances inspection as the evaluation indexes,the feasibility of the impurity removal method was definited and the process parameters were optimized.Results The optimized process parameters were as follows: refrigerated for 24 h,centrifugated for 15 min,at 5 000 r/min,activated carbon dosage of 0.3%,temperature 40 ℃,adsorption time 30 min,and the original solution pH value.Conclusion The impurity removal effect of refrigeration,centrifugation,and activated carbon adsorption is significant,which could effectively remove the resin,protein,and other impurities.

OBJECTIVE:To establish an HPLC method for simultaneous determination of contents of loureirin A, loureirin B, 7,4'-dihydroxy flavone, pterostilbene and resveratrol in resina draconis and its extracts.METHOD:Kromasil 100-5C18 column (4.6 mm x 250 mm, 5 microm) was used with the mobile phase of acetonitrile-1% glacial acetic acid at a flow rate of 1.0 mL x min(-1) and the column temperature at 40 degrees C. The detective wave length of loureirin A and B was detected at 278 nm, and 7,4'-dihydroxy flavone, pterostilbene and resveratrol was at 319 nm.RESULT:All the five active components reached the resolved peaks within 40 min, indicating a good linearity (r > or = 0.999 7). The average recoveries of loureirin A, loureirin B, 7,4'-dihydroxy flavone, pterostilbene and resveratrol in resina draconis were 102.9%, 96.81%, 97.29%, 100.7% and 103.7%, with RSDs of 0.23%, 1.5%, 0.42%, 0.58% and 0.34%, respectively. The average recoveries of loureirin A, loureirin B, 7,4'-dihydroxy flavone, pterostilbene and resveratrol in extract of resina draconis were 102. 2% , 96. 93%, 97. 90% , 102.0% and 103.3%, with RSDs of 1.7%, 0.91%, 1.4%, 1.5% and 1.2%, respectively.CONCLUSION:The method is so easy, accurate, highly repeatable and stable that it provides good reference for the quality control of resina draconis and its extracts.

目的 对二至丸处方提取物的醋酸乙酯萃取部位和水饱和正丁醇萃取部位进行化学成分研究.方法 采用柱色谱法进行分离和纯化,经过波谱分析进行结构鉴定.结果 从二至丸处方提取物的醋酸乙酯和水饱和正丁醉部位共分离得到11个单体化合物,分别鉴定为齐墩果酸(1)、熊果酸(2)、木犀草素(3)、芹菜素(4),槲皮素(5)、特女贞苷(6)、蟛蜞菊内酯(7)、去甲蟛蜞菊内酯(8)、甘露醇(9)、女贞苷G13(10)和木犀榄苷二甲酯(oleoside dimethyl ester,11).结论 化合物1～11均为首次从该复方中得到.