E89684E5B182E5B182E69E90.docVIP

薄层层析-紫外分光光度法测定香丹注射液中原儿茶醛的含量 【摘要】? 目的? 建立薄层层析-紫外分光光度法测定香丹注射液中原儿茶醛的含量。? 以原儿茶醛为对照品，展开剂为二氯甲烷-乙酸乙酯-甲酸（85∶0.8）分离得到原儿茶醛，采用紫外分光光度法，检测波长281nm，测定原儿茶醛的含量。结果? 原儿茶醛在0.55～4.95μg/ml 范围内线性关系良好，r=0.9998。平均含量为0.174mg/ml，加样回收率为97.3%～102.3%，RSD为1.6%。结论? 实验结果表明，薄层层析-紫外分光光度法测定香丹注射液中原儿茶醛的含量，方法操作简便，准确度高，精密度好，可作为样品的检测方法。??? ??? 【关键词】? 香丹注射液；原儿茶醛；薄层层析-紫外分光光度法；含量测定??????????????? 【Abstract】? Objective? A TLC-UV method was developed to separate and determine protocatechuic aldehyde in injection saliae miltiorrhizae composita.Methods? Contrasting with protocatechuic aldehyde， the amount of protocatechuic aldehyde in injection saliae miltiorrhizae composita have been determined by TLC-UV with methylene chloride-acetic acid acetic ester-formic acid（85∶0.8）as the developing solvent and the detection wavelength at 281nm.Results? calibration carver was linear in the range of 0.55～4.95μg /ml (r=0.9998)for protocatechuic aldehyde .The average amount is 0.174mg /ml.The recoveries of protocatechuic aldehyde are between 97.3% and 102.3%，and RSD% was not more than 2.0%.Conclusion? The method is simple，rapid and reproducible for determination of protocatechuic aldehyde in injection saliae miltiorrhizae composita.??? ??? 【Key words】? injection of saliae miltiorrhizae composita；protocatechuic aldehyde；TLC-UV；content determination??? ??? 香丹注射液为棕色澄明液体，是由降香和丹参提取物配制而成，临床用于心绞痛、心肌梗死等。处方中降香是豆科植物降香檀树干和根的干燥心材，性辛，温，能活血止血，行气止痛。丹参为唇形科植物丹参的干燥根及根茎，性微寒味苦，具有活血化瘀，凉血消肿，清心除烦之功效。丹参的化学成分［1］为两类，一类为脂溶性的二萜醌类，主要为丹参酮和丹参酮Ａ，具有抗菌、抗炎及扩张血管作用；另一类为水溶性的酚酸类，主要为原儿茶醛，是抗心绞痛有效成分。中华人民共和国药品卫生部药品标准WS3-B-3289-98采用高效液相色谱法测定香丹注射液中原儿茶醛的含量［2］。本文有关［3，4］建立了薄层层析-紫外分光光度法分离测定香丹注射液中原儿茶醛的含量，方法简便，准确度高，精密度好，成本低廉。??? ??? 1? 材料与仪器??? ??? 1.1? 材料? 二氯甲烷、乙酸乙酯、甲酸，均为纯。对照品：原儿茶醛（药品生物制品检定所）。薄层层析硅胶G（青岛海洋化工有限公司）化学纯。水为蒸馏水。香丹注射液（10ml/支）。??? ??? 1.2? 仪器? 752紫外可见分光光度计（上海菁华仪器有限公司）。微量点样器（5μl）。分析天平。??? ??? 2? 实验方法??? ??? 2.1? 薄层层析条件的考察??? ??? 2.1.1? 对照品溶液的制备? 精密称取原儿茶醛对照品1.1mg，置10ml容量瓶中，加水溶解稀释至刻度，摇匀即得浓度为0.11mg/ml。??? ??? 2.1.2? 阴性对照品溶液的制备? 取降香10g加水100ml浸润，进行水蒸