基于HPLC法考察5种赋形剂对双柏散制成糊剂有效成分的影响  

The Effect of Five Excipients on the Effective Ingredients of Shuangbai Powder(双柏散)Paste Based on HPLC

作　　者：蓝鲜艳 张洪平 卢鲜云 郑厚平 梁学政 LAN Xianyan;ZHANG Hongping;LU Xianyun;ZHENG Houping;LIANG Xuezheng(Liuzhou Hospital of Traditional Chinese Medicine,Liuzhou Guangxi 545001,China)

机构地区：[1]柳州市中医医院,广西柳州545001

出　　处：《中医药导报》2022年第7期55-58,共4页Guiding Journal of Traditional Chinese Medicine and Pharmacy

基　　金：广西自然科学基金项目(2020GXNSFBA297112);柳州市科技局资助项目(2019DH10604)。

摘　　要：目的:探讨不同辅料调制双柏散制成糊剂的甲醇提取液中大黄素、小檗碱的含量变化。方法:建立HPLC法,色谱柱为Poroshell 120 EC-C_(18)(4.6 mm×150 mm,4μm),检测波长为275 nm,乙腈为流动相A,0.4%磷酸水为流动相B,梯度洗脱,流速为1 mL/min,柱温为26℃,测定水、蜂蜜水、姜汁、白糖水、醋5种赋形剂调制双柏散成糊剂甲醇提取液中小檗碱、大黄素的含量。结果:双柏散供试品溶液与混合对照品溶液中小檗碱、大黄素的积分峰一一对应,专属性良好;样品中小檗碱、大黄素与相邻色谱峰完全分离,大黄素、小檗碱进样浓度与峰面积呈良好的线性关系,线性方程为:y_(小檗碱)=21614x-14.509(r=0.9997,浓度范围0.0088~0.0352 mg/mL),y_(大黄素)=32223x-4.0547(r=0.9994,浓度范围0.0022~0.0086 mg/mL);精密度、稳定性、重复性试验的RSD<2%;小檗碱、大黄素平均回收率分别为97.96%(RSD=0.61%)、96.05%(RSD=0.66%)。小檗碱各组含量排序为水调组>糖水组>蜂蜜组=醋调组>姜汁组;大黄素各组含量排序为蜂蜜组>水调组>姜汁组>糖水组>醋调组。结论:本研究建立的高效液相色谱法能够同时测定双柏散方中大黄素、小檗碱有效成分,方法操作方便、快速、可行性好;双柏散以水作赋形剂时小檗碱、大黄素含量相对较高。Objective:To investigate the content changes of emodin and berberine in methanol extract of Shuangbai powder paste prepared with different excipients.Methods:HPLC method was established.The chromatographic column was Poroshell 120 EC-C_(18)(4.6 mm×150 mm,4μm).The detection wavelength was 275 nm.Acetonitrile was the mobile phase A and 0.4%phosphoric acid water was the mobile phase B.With gradient elution,the flow rate was 1 mL/min and the column temperature was 26℃.The contents of berberine and emodin in the methanol extract of Shuangbai powder paste prepared with five excipients,including water,honey water,ginger juice,sugar water and vinegar,were determined.Results:The integral peaks of berberine and emodin in Shuangbai powder test solution and mixed reference solution corresponded one by one,and the specificity was good;Berberine and emodin in the sample were completely separated from the adjacent chromatographic peaks,and the injection concentration of emodin and berberine showed a good linear relationship with the peak area.The linear equation is as follows:y(berberine)=21614x-14.509(r=0.9997,concentration range 0.0088-0.0352 mg/mL),y(emodin)=32223x-4.0547(r=0.9994,concentration range 0.0022-0.0086 mg/mL).RSD of precision,stability and repeatability experiments was less than 2%.The average recoveries of berberine and emodin were 97.96%(RSD=0.61%)and 96.05%(RSD=0.66%)respectively.The content of berberine in each group was ranked as water conditioning group>sugar water group>honey group=vinegar conditioning group>ginger juice group;The content of emodin in each group was ranked as honey group>water conditioning group>ginger juice group>sugar water group>vinegar conditioning group.Conclusion:The HPLC method established in this study can simultaneously determine the effective components of emodin and berberine in Shuangbai power prescription.The method is convenient,rapid and feasible.The contents of berberine and emodin in Shuangbai powder were relatively high when water was used as excipient.

关 键 词：双柏散 糊剂 赋形剂 小檗碱 大黄素 高效液相色谱 

分 类 号：R284.1[医药卫生—中药学]