粉碎过筛条件对吴茱萸含量测定结果的影响及解决办法

目的研究不同的粉碎过筛条件对吴茱萸含量测定的影响规律,提出能反映取样代表性的粉碎过筛方法,以减小实验误差。方法以绿原酸、金丝桃苷、去氢吴茱萸碱、吴茱萸碱、吴茱萸次碱和吴茱萸新碱为指标,采用HPLC法测定不同粉碎过筛条件对其含量测定的影响。通过比较不同条件下各指标成分的含量及分析结果的精密度,剖析粉碎过筛影响含量测定结果的原因,进而确定合适的粉碎过筛方法。结果吴茱萸中6种活性成分的含量与内果皮在粉末中的比例呈负相关。按《中国药典》2015年版方法处理样品,6种活性成分含量测定的日内精密度和重复性试验结果多数不符合要求(RSD5.0%)。当所有粉末都过2号筛时,分析结果的精密度和重复性都符合分析要求(RSD2.0%)。结论内果皮等纤维素颗粒在粉末中的比例是药材粉碎过筛环节最关键的影响因素。所有粉末都能过2号筛的粉碎过筛方式既保证了取样的代表性,又解决了分析结果的精密度和准确度符合分析要求的问题。

Effects of crushing and sieving on compounds contents of Euodiae Fructus and its solution

Objective To study the effect factors and rules of the different crushing and sieving methods on the compounds contents of Euodiae Fructus(EF), and to propose an optimized crushing and sieving method which can reflect the sampling representativeness and reduce errors.Methods The bioactive compounds such as chlorogenic acid, hyperoside, dehydroevodiamine, evodiamine, rutaecarpine, and evocarpine were selected as the evaluation markers.The effects of the different crushing and sieving conditions were evaluated by comparing the contents and analytical precisions of EF components under different conditions by HPLC.The influencing factors and the rules were discussed and the suitable crushing and sieving method was then proposed.Results The contents of six components in EF were negatively correlated with the proportions of the endocarps in powders.Most intraday and intermediate precisions of six bioactive compounds don''t meet the standards using the current pharmacopoeia method with RSD > 5%.And when all powders passing through 2^# sieve, the good analytical precision and repeatability were obtained with RSD < 2%.Conclusion The cellulose particles, such as endocarps, are the key factors during the crushing and sieving process of the herbs.The crushing and sieving method with all powders passing through 2^# sieve not only ensures the sampling representativeness, but also solves the analytical precision and accuracy.