益母草当归锭的制备及主成分阿魏酸含量测定

Preparation of Yimucao Danggui tablets and content determination of ferulic acid

为确定益母草当归锭的制备工艺,并制定益母草当归锭主要成分阿魏酸的含量限度,本试验以益母草和当归为原料,将其超微粉碎后得到微粉,加入黏合剂,通过湿法制粒得到软材,再经过制粒、整粒、压片等步骤,制得益母草当归锭;采用高效液相色谱法对阿魏酸含量检测方法的专属性、线性、重复性、精密度、耐受性以及加样回收试验等方法学进行考察,并通过对制备的10批样品进行检测,建立益母草当归锭中阿魏酸的含量检测方法及限度。结果显示,制得的益母草当归锭为表面光滑的圆柱状,每锭质量达120 g;阿魏酸的高效液相色谱检测方法专属性、线性、重复性、精密度、耐受性以及加样回收试验结果均良好;测得10批样品中阿魏酸的含量为0.34~0.52 mg/g,考虑到当归药材的产地、来源、炮制加工、生产及贮存等因素对阿魏酸含量的影响,将阿魏酸含量限度在最小值的基础上下降10%,暂定阿魏酸含量不得少于0.31 mg/g,作为益母草当归锭的含量检测限度。结果表明,本试验益母草当归锭制备方法简单,每锭载药量大,1锭即可达到治疗剂量,方便投喂,建立的阿魏酸高效液相色谱含量检测方法稳定、可行,可用于益母草当归锭的质量控制。

The objective was to study the preparation process of Yimucao Danggui tablets,and establish the content limit of ferulic acid.In this experiment,Herba Leonuri and Radix Angelicae Sinensis were used as raw materials,and ultrafine powders were obtained after crushing.Appropriate adhesives were added to obtain soft materials through wet granulation.Then,Yimucao Danggui tablets were prepared through steps such as granulation,whole granulation,and tablet pressing.The content of ferulic acid in Yimucao Danggui tablets was determined by high-performance liquid chromatography,the specificity,linearity,repeatability,precision,tolerance,sample recovery and other methodological aspects of the detection method were tested.Limit for ferulic acid content determination in Yimucao Danggui tablets was determined by detecting 10 batches of prepared samples.The results showed that the surface of the prepared Yimucao Danggui tablets was smooth and cylindrical,with a weight of 120 g per ingot.The specificity,linearity,repeatability,precision,tolerance,and sample recovery test results of the method for ferulic acid were good.The content of ferulic acid in 10 batches of samples was 0.34-0.52 mg/g.Considering factors such as the origin of the medicinal material,processing,production and storage,the quality requirement was reduced by 10%from the minimum value.Therefore,the content of ferulic acid should not be less than 0.31 mg/g,which is used for the content detection limit of Yimucao Danggui tablets.It is concluded that the method of preparing Yimucao Danggui tablets is simple,with a large drug loading capacity per tablet.One tablet can reach the therapeutic dose.The established method for detecting the content of ferulic acid by high-performance liquid phase is stable and feasible,and can be used for quality control of Yimucao Danggui tablets.