芎附滴丸的制备工艺及主要成分的含量测定研究

Study on the preparation technique and content determination of the main components in Xiongfu Dripping Pills

目的:确立芎附滴丸的制备工艺,并建立一种同时检测芎附滴丸中6种主要成分的含量测定方法,为芎附滴丸的质量控制提供依据。方法:按照芎附提取物与PEG 6000=1 2比例水浴加热熔融,搅拌均匀后倾入滴丸机中,滴丸在二甲基硅油中冷却固化成丸,取出,吸干冷却剂,制得芎附滴丸。对芎附滴丸进行外观形状、重量差异、溶散时限检查。采用Kromasil-C18(250mm×4.6mm,5μm)色谱柱,甲醇-0.1%甲酸溶液为流动相,梯度洗脱,体积流量1.0mL/min,柱温25℃,测定芎附滴丸中6种主要成分含量。结果:所制芎附滴丸外观形状、重量差异、溶散时限均符合《中华人民共和国药典》要求。建立的HPLC法可同时测定芎附滴丸中阿魏酸、洋川芎内酯Ⅰ、洋川芎内酯A、Z-藁本内酯、香附烯酮和α-香附酮的含量,该方法精密度、重复性、稳定性良好,各成分平均加样回收率和相应的RSD分别为102.11%(2.16%)、99.78%(2.25%)、101.52%(2.06%)、97.93%(2.64%)、100.93%(2.43%)、102.29%(2.72%)。结论:芎附滴丸制备工艺简便可行,所建立的含量测定方法简单、快速、准确,可为芎附滴丸的质量控制提供科学依据。

Objective:To establish a preparation technique and develop a method for simultaneous determination of six components in Xiongfu Dripping Pills,and to provide scientific basis for the quality control of Xiongfu Dripping Pills.Methods:The extract and PEG 6000 were melted in a water bath at a ratio of 1:2,stirred,and poured into the dripping pill machine.The dripping pills were cooled and solidified in the dimethyl silicone oil.The dripping pills were taken out and the coolant on the surface was cleaned up.The product character,weight difference and the time limit of dissolve were examined.The chromatographic separation was achieved on a Kromasil-C18(250 mm×4.6 mm,5μm)column with methanol-0.1%formic acid solution as mobile phases at the flow rate of 1.0 mL/min for gradient elution.The column temperature was 25℃.Six main components were determined.Results:The product character,weight difference and the time limit of dissolve met the requirements of the Pharmacopoeia of the People’s Republic of China.The HPLC-DAD method determined the content of ferulic acid,senkyunolideⅠ,senkyunolide A,Z-ligustilide,cyperotundone andα-cyperone.The precision,repeatability and stability were good.The average recoveries and corresponding RSD values were 102.11%(2.16%),99.78%(2.25%),101.52%(2.06%),97.93%(2.64%),100.93%(2.43%),102.29%(2.72%),respectively.Conclusion:The preparation technique is simple and feasible.The HPLC method is simple,quick,accurate,and it can provide scientific basis for the quality control of Xiongfu Dripping Pills.