大黄[庶虫]丸中17种质量标志物的含量测定

Content Determination of 17 Quality Markers in Dahuang Zhechong Pills

目的:建立同时测定大黄[庶虫]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[庶虫]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Kromasil 100-5-C18(250 mm×4.6mm,5μm),流动相为0.1%磷酸溶液-乙腈(梯度洗脱),流速为1.0 m L/min,柱温为30℃,检测波长为210 nm,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/m L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?虫丸的质量标准。

OBJECTIVE:To establish the method for the content determination 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,5μm)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 20μL.RESULTS:The linear range of above 17 quality markers were5.74-183.53,6.51-208.24,4.30-137.65,4.60-147.06,4.12-131.76,4.25-135.88,6.31-201.76,4.60-147.06,1.94-62.06,4.47-142.94,0.69-22.06,2.29-73.24,2.33-74.41,1.42-45.29,6.65-212.94,1.11-35.44 and 1.47-47.06μg/m L,respectively(all R2≥0.9990).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.