复方桔梗止咳片中远志、甘草的含量测定及质量情况分析

Content Determination and Quality Analysis of Polygalae Radix and Glycyrrhizae Radix et Rhizoma in Fufang Jiegeng Zhike Pian

目的:建立复方桔梗止咳片中远志(3,6’-二芥子酰基蔗糖)和甘草(甘草酸)中成分的含量测定方法,了解复方桔梗止咳片的整体质量情况,保障公众用药安全有效。方法:采用HPLC,MG C18色谱柱(4. 6 mm×250 mm,5μm),流动相乙腈-0. 05%磷酸水溶液(18∶82)检测远志(3,6’-二芥子酰基蔗糖),(35∶65)检测甘草(甘草酸),进样量20μL,柱温30℃,流速1. 0 m L·min-1,检测波长320 nm检测远志(3,6’-二芥子酰基蔗糖),250 nm检测甘草(甘草酸)。结果:3,6’-二芥子酰基蔗糖在0. 105 8~2. 643 8μg呈良好的线性关系(r=0. 999 5),甘草酸在0. 077 0~5. 773 0μg呈良好的线性关系(r=1. 000 0),3,6’-二芥子酰基蔗糖和甘草酸的平均回收率分别为96. 2%和95. 6%,RSD分别为1. 2%和0. 9%;通过对178批样品中远志和甘草成分的含量测定,发现部分生产企业存在不投、少投或用劣质药材(饮片)投料现象,且不同生产企业、同一企业不同批号之间的质量情况差异较大。结论:该方法简便、准确、重复性好、灵敏度高,为复方桔梗止咳片的全面质量控制提供了科学依据。

Objective:To establish the method for determining the content of Polygalae Radix(3,6’-disinapoylsucrose)and Glycyrrhizae Radix et Rhizoma(glycyrrhizic acid)in Fufang Jiegeng Zhike Pian,so as to know the overall quality condition of Fufang Jiegeng Zhike Pian and ensure the safety and effectiveness of public medication.Method:HPLC was performed of MG C18 chromatographic column(4.6 mm×250 mm,5μm)and mobile phase acetonitrile-0.05%phosphoric acid solution were used to test Polygalae Radix(3,6’-disinapoylsucrose)and Glycyrrhizae Radix et Rhizoma(glycyrrhizic acid),with the sample amount of 20μL,flow rate of 1.0 m L·min-1,and column temperature of 30℃,where the mobile phase acetonitrile-0.05%phosphoric acid solution and detection wavelength were 18∶82 and 320 nm for Polygalae Radix(3,6’-disinapoylsucrose)and 35∶65 and 250 nm for Glycyrrhizae Radix et Rhizoma(glycyrrhizic acid).Result:3,6’-Disinapoylsucrose and glycyrrhizic acid presented high linearity with the peak area at 0.105 8-2.643 8μg(r=0.999 5)and 0.077 0-5.773 0μg(r=1.000 0)respectively,and the average recovery rate was 96.2%(RSD1.2%)and 95.6%(RSD 0.9%).After content determination of Polygalae Radix and Glycyrrhizae Radix et Rhizoma in 178 batches of samples,it was found that some producers input no,only a few or even poor medicinal materials(medicinal slices)during production,and the quality varied a lot among products from different producers and products of different batches from a same producer.Conclusion:The method is simple,accurate,and highly reproducible and sensitive,providing scientific basis for the overall quality control of Fufang Jiegeng Zhike Pian.