大黄䗪虫丸中17种质量标志物的含量测定
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篇名: 大黄䗪虫丸中17种质量标志物的含量测定
TITLE: Content Determination of 17 Quality Markers in Dahuang Zhechong Pills
摘要: 目的:建立同时测定大黄䗪虫丸中17种质量标志物含量的方法。方法:采用高效液相色谱(HPLC)法测定10批市售大黄䗪虫丸中尿囊素、次黄嘌呤、红景天苷、羟基芍药苷、甘草苷、异甘草苷、黄芩苷、对甲氧基苯乙酸、汉黄芩苷、肉桂酸、芹菜素、柚皮素、去甲汉黄芩素、芦荟大黄素、大黄酸、白杨素、大黄素等17种质量标志物的含量。色谱柱为Kromasil100-5-C18(250mm×4.6mm,5μm),流动相为0.1%磷酸溶液-乙腈(梯度洗脱),流速为1.0mL/min,柱温为30℃,检测波长为210nm,进样量为20μL。结果:上述17种质量标志物的质量浓度依次在5.74~183.53、6.51~208.24、4.30~137.65、4.60~147.06、4.12~131.76、4.25~135.88、6.31~201.76、4.60~147.06、1.94~62.06、4.47~142.94、0.69~22.06、2.29~73.24、2.33~74.41、1.42~45.29、6.65~212.94、1.11~35.44、1.47~47.06μg/mL范围内与各自峰面积呈良好的线性关系(R2均不小于0.9990)。该方法精密度、重复性、稳定性、耐用性的RSD均小于2%(n=6);17种质量标志物的平均加样回收率范围为96.31%~101.73%,RSD均小于3%(n=6)。结论:本方法简便、快速,专属性、精密度、重复性、稳定性、准确度和耐用性均良好,可用于完善大黄䗪虫丸的质量标准。
ABSTRACT: OBJECTIVE:To establish the method for the content de termination of 17 quality markers in Dahuang zhechong pills(DHZCP). METHODS :HPLC method was adopted to determine the contents of 17 quality markers in 10 batches of DHZCP , such as allantoin ,hypoxanthine,salidroside,hydroxypaeoniflorin,glycyrrhizin,isoglycyrrhizin,baicalin,p-methoxyphenylacetic acid,wogonin,cinnamic acid ,apigenin,naringin,norwogonin,aloe emodin ,rhein,chrysin,emodin. The determination was performed on Kromasil 100-5-C18(250 mm × 4.6 mm,5 μm)column with mobile phase consisted of 0.1% phosphoric acid solution-acetonitrile (gradient elution ) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃ ,the detection wavelength was 210 nm and the sample size was 20 μ L. RESULTS:The linear range of above 17 quality markers were 5.74-183.53,6.51-208.24,4.30-137.65,4.60-147.06,4.12-131.76,4.25-135.88,6.31-201.76,4.60-147.06,1.94-62.06,4.47- 142.94,0.69-22.06,2.29-73.24,2.33-74.41,1.42-45.29,6.65-212.94,1.11-35.44 and 1.47-47.06 μg/mL,respectively(all R2≥ 0.999 0). RSDs of precision ,repeatability,stability and durability tests were all less than 2%(n=6);average recovery of 17 quality markers ranged from 96.31% to 101.73%,and the RSDs were less than 3%(n=6). CONCLUSIONS :The method is simple, rapid,speific,specise,reproducible,stable,accurate and durable ,and can be used for improving the quality standard of DHZCP.
期刊: 2021年第32卷第19期
作者: 付传奎,许珂嘉,张子蒙,黄艳,陈志鹏,李伟东,吴丽
AUTHORS: FU Chuankui ,XU Kejia,ZHANG Zimeng ,HUANG Yan,CHEN Zhipeng ,LI Weidong ,WU Li
关键字: 大黄䗪虫丸;质量标志物;高效液相色谱法;质量标准;含量测定
KEYWORDS: Dahuang zhechong pills ;Quality marker ;HPLC;Quality stan dard;Content determination
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