分散液液萃取-HPLC测定中药化妆品中皂苷含量

Dispersive Liquid-Liquid Extraction Coupled with HPLC for the Determination of Saponins in Chinese Medicine Cosmetics

关键词:  分散液液萃取法(DLLE)  中药化妆品  中药活性成分  快速除杂

Key words:  dispersive liquid-liquid extraction(DLLE)  Chinese medicine cosmetics  active ingredients in Chinese medicine  rapid removal of impurity

摘要:

目的 建立一种简便快速的分散液液萃取法（dispersive liquid-liquid extraction method，DLLE）用于除去中药化妆品中的基质类干扰成分，分离得到目标活性成分，并进行含量测定。方法 取样品加甲醇溶解，过滤，调pH值至酸性。精密量取滤液1.0 mL，加入3 mL水饱和的氯仿和0.5 mL水，涡旋振荡2 min使成均一的乳浊液。离心（3 000 r·min^-1，5 min）分取上清液，即可完成中药化妆品中基质成分的去除以及目标活性成分的纯化。结果 使用DLLE法对中药化妆品进行处理，分离得到活性成分，方法回收率为97.3%~98.0%，精密度和重复性良好。样品测定3个批号的中药护肤霜中人参皂苷Rg1含量测定值分别为0.236，0.210，0.222 mg·g^-1。结论 本研究所建立的DLLE法操作简便，能快速有效地去除中药化妆品中的基质干扰，分离得到目标成分，方法回收率高；有机溶剂用量少，为中药化妆品分析测定提供了一个很好的分析手段。

Abstract:

OBJECTIVE To establish a simple and rapid dispersive liquid-liquid extraction method (DLLE) to remove the stromal interference components in traditional Chinese medicine cosmetics, so as to isolate the target active components, and to determine the isolated content. METHODS Sample was dissolved in methanol, then the sample solution was filtered and the filtrate pH was adjusted to acidic. The 1.0 mL filtrate was measured precisely into a centrifuge tube, then 3 mL chloroform which was saturated with water and 0.5 mL water were added successively. Subsequently, the mixture was vortexed for 2 min to form a homogeneous emulsion. Then the cloudy solution was centrifuged for 5 min, and the supernatant was collected. As a result, the removal of impurity and the seperation of target content were both accomplished. RESULTS By using the DLLE method for pretreatment of cosmetics sample, targeted active ingredient was isolated, and the recovery of method was between 97.3% to 98.0%, and the methed has good precision and repeatability. The saponins values that was measured in three batches of dermatological Chinese medicine cosmetics were 0.236, 0.210, 0.222 mg·g^-1, respectively. CONCLUSION The DLLE method developed in this paper is simple, and can effectively eliminate the interference and isolate targeted ingredient. In addition the methed has high recovery rate,low organic solvent consumption and thus provides a good analysis method for the determination of saponins in Chinese medicine cosmetics.