薯莨的质量控制方法

Quality Control Method for Dioscorea cirrhosa

目的:建立中药薯莨的质量控制方法,提高其质量可控性。方法:采用显微鉴别法对薯莨的粉末显微特征进行鉴别,薄层色谱法(TLC)对薯莨进行薄层色谱鉴别,高效液相色谱法(HPLC)测定薯莨中儿茶素和表儿茶素含量,参考2015年版《中国药典》四部通则测定10批薯莨的水分、总灰分、酸不溶性灰分和醇溶性浸出物含量。结果:薯莨粉末显微特征明显,具有草酸钙针晶、淀粉粒和石细胞等。薄层色谱鉴别显示薯莨中主斑点分离较好,斑点颜色及Rf值与对照药材一致。HPLC结果显示薯莨药材中的儿茶素和表儿茶素分离度好,线性范围分别是4.900~196.0,5.020~200.8mg·L^-1,相关系数r均为0.9999。精密度、重复性和稳定性良好,平均加样回收率分别为99.67%和99.25%,RSD分别为1.5%和1.6%。不同批次薯莨中儿茶素和表儿茶素的含量范围分别为0.5532~10.25mg·g^-1和0.6461~11.06mg·g^-1。10批水分质量分数平均值为16.3%,总灰分质量分数平均值为3.97%,酸不溶性灰分平均值为1.41%,醇溶性浸出物平均质量分数为20.3%:结论:该方法简便、准确、可靠,可以为更有效的控制薯莨的质量提供参考依据。

Objective:To establish a systematic quality control method for Dioscorea cirrhosa and improve its quality controllability.Method:Microscopic identification method was applied to identify the powder microscopic characteristics of D.cirrhosa;and thin layer chromatography (TLC)was applied to identify its thinlayer chromatography,and high performance liquid chromatography (HPLC)was employed to determinate the contents of catehin and epicatechin in D.cirrhosa.The contents of water,total ash,acid insoluble ash and alcohol-soluble extractives were measured based on Chinese Pharmacopoeia 2015 version.Result:The obvious microscopic characteristics,such as needle-like calcium oxalate crystals,starch granules and stone cells were observed.The spots in TLC chromatograms of D.cirrhosa were clear,with spot color and Rf value consistent with those of the controls HPLC results showed that catehin and epicatechin were well separated and there were good linear relationships (r =0.9999)at the ranges within 4.900-196.0,5.020-200.8mg·L^-1 respectively.The average recoveries of catehin and epicatechin were 99.67% and 99.25%,respectively,RSDof 1.5%and 1.6% respectively,with a high precision,repeatability and stability.The contents of catehin and epicatechin were in the range of 0.5532-10.25mg ·g^-1and 0.6461-11.06mg·g^-1in different batches of D.cirrhosa.The average mass fraction of water,total ash,acid insoluble ash and alcohol-soluble extractives were 16.3%,3.97%, 1.41% and 20.3%,respectively in 10batches of samples.Conclusion:The method was simple,accurate and reliable,and can provide reference and basis for more effective quality control of D.cirrhosa.