参黄排毒灌肠剂质量控制研究  

Study on Quality Control of Shenhuang Detoxification Enema

作　　者：陈晓铤 钟昶国 熊艳丽 陈健明 柯颖标 刘舒雅 陈洪毅 Chen Xiao-ting;Zhong Chang-guo;Xiong Yan-li;Chen Jian-ming;Ke Ying-biao;Liu Shu-ya;Chen Hong-yi(Pharmacy Department,Maoming Hospital of Traditional Chinese Medicine,Maoming 525000,China;Guangdong Laboratory Animails Monitoring Institute,Guangzhou 510663,China)

机构地区：[1]茂名市中医院,广东茂名525100 [2]广东省实验动物监测所,广东广州510663

出　　处：《北方药学》2024年第3期1-4,共4页Journal of North Pharmacy

摘　　要：目的:采用薄层色谱和高效液相色谱对参黄排毒灌肠剂中的大黄和丹参分别进行定性和定量的鉴别,用于医院中灌肠剂的质量保障,更有效的治疗患者。方法:薄层色谱采用硅胶G薄层板,以大黄、丹参对照药材和大黄酚、丹参素钠为对照,对薄层色谱特征点进行对比;高效液相色谱采用Kromasi lC18色谱柱(4.6 mm×250 mm,5μm)进行分析,其中,大黄酸、大黄酚的流动相为甲醇-0.1%磷酸溶液(85:15),检测波长为254 nm,丹参酮I、丹参酮IIA、隐丹参酮的流动相为乙腈-0.02%磷酸溶液(61:39),梯度洗脱,检测波长为270 nm,流速为1.0mL/min,柱温为30℃。结果:参黄排毒灌肠剂的色谱斑点分离度好,大黄、丹参的特征斑点清晰,与对照品特征点一致;大黄酸、大黄酚、丹参酮I、丹参酮IIA、隐丹参酮在各自范围内与峰面积线性关系良好(r≥0.99),加样回收率为96.88%~108.28%,RSD为0.79%~2.76%,大黄酸、丹参酮I的平均含量分别为(22.15±0.42)μg/mL、(40.20±1.26)μg/mL。结论:此次方法可以多次应用,结果具有准确和一致性,我们拟定了参黄排毒灌肠剂中大黄酸和丹参酮I的含量分别不能低于15μg/mL、30μg/mL的标准,用于参黄排毒灌肠剂的质量控制。Objective:To identify the rhubarb and salvia miltiorrhiza in Shenhuang detoxification enema by TLC and HPLC,to ensure the quality of enema in hospital and treat patients more effectively.Method:TLC uses silica gel plates,n-hexane-ethyl acetate-formic acid(40:10:0.5)and chloroform-acetone-formic acid(25:10:4)was the developing agent for Rhubarb and Salvia miltiorrhiza,respectively.And Rhubarb and Salvia miltiorrhiza as the reference medicinal materials,Chrysophanol and Sodium danshensu as the controls to compare the characteristic points of TLC.HPLC analyzed using a Kromasi lC18 chromatographic column(4.6 mm×250 mm,5μm).The mobile phase of Rhein and Chrysophanol was methanol-0.1%phosphoric acid solution(85:15),the detection wavelength was 254 nm.The mobile phase of Tanshinone I,TanshinoneⅡA and Cryptotanshinone was acetonitrile-0.02%phosphoric acid solution(61:39),gradient elution,the detection wavelength is 270 nm.And the flow rate is 1.0mL/min,and the column temperature is 30°C.Results:The chromatographic spot separation of Shenhuang detoxification enema is good,and the characteristic spots of Rhubarb and Salvia miltiorrhiza are clear and consistent with the characteristic spots of the reference substance.Rhein,Chrysophanol,Tanshinone I,TanshinoneⅡA and Cryptotanshinone have a good linear relationship with the peak area within their respective ranges(r≥0.99),the average recovery rate of the added sample is 96.88%~108.28%,the RSD is 0.79%~2.76%,and the average content of Rhein and Tanshinone I are(22.15±0.42)μg/mL,(40.20±1.26)μg/mL,respectively.Conclusion:This method has accurate results and good repeatability,we have formulated standards that the contents of Rhein and Tanshinone I in Shenhuang detoxification enema should not be less than 15μg/mL and 30μg/mL,respectively,for quality control of Shenhuang detoxification enema.

关 键 词：参黄排毒灌肠剂 薄层色谱 高效液相色谱 大黄 丹参 质量控制 

分 类 号：R692.5[医药卫生—泌尿科学]