摘要
目的:采用HPLC法,建立杏苏止咳颗粒指纹图谱和7种成分定量分析的测定方法,为杏苏止咳颗粒的质量控制提供更为可靠的方法和依据。方法:采用HPLC法,同时测定杏苏止咳颗粒中苦杏仁苷、甘草苷、橙皮苷、迷迭香酸、甘草酸铵、白花前胡甲素、白花前胡乙素的含量,采用ZORBAX Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.01%磷酸溶液,梯度洗脱;检测波长为250 nm、320 nm,柱温为30℃,流速为1.0 ml·min^-1,进样量为10μl。选取橙皮苷为参照峰,并使用中药色谱指纹图谱相似度评价系统对指纹图谱进行相似性评价,确定共有峰,并采用SPSS 22.0软件对含量测定结果进行聚类分析。结果:苦杏仁苷、甘草苷、橙皮苷、迷迭香酸、甘草酸铵、白花前胡甲素、白花前胡乙素检测质量浓度的线性范围分别为4.515~63.210μg·ml^-1(r=0.9996),0.488~6.829μg·ml^-1(r=0.9998),2.288~32.030μg·ml^-1(r=0.9995),0.390~5.461μg·ml^-1(r=0.9997),1.781~24.930μg·ml^-1(r=0.9996),1.321~18.490μg·ml^-1(r=0.9994),0.378~5.288μg·ml^-1(r=0.9996)μg·ml^-1;平均加样回收率分别为98.6%,98.5%,99.0%,98.7%,99.1%、98.7%,98.5%(RSD<2.0%,n=6)。12批杏苏止咳颗粒的指纹图谱与其指纹图谱共有模式相比较相似度均大于0.9,标定了共有峰22个,并对其中7个共有指纹峰进行了指认和归属。通过聚类分析,12批样品聚成2类。结论:所建立的HPLC指纹图谱分离效果良好,特征性强,方法稳定简单,多指标成分含量测定同时结合指纹图谱分析能更为全面地对杏苏止咳颗粒的质量进行控制。
Objective:To establish a method for the qualitative analysis of fingerprints and the quantitative analysis of 7 components of Xingsu Zhike granules by HPLC to provide a more reliable method and basis for the quality control of Xingsu Zhike granules.Methods:The determination was performed on a ZORBAX Eclipse XDB C18 column(250 mm×4.6 mm,5μm)with the mobile phase consisting of acetonitrile-0.01%phosphoric acid(gradient elution)at the flow rate of 1.0 ml·min^-1.The detection wavelengths were set at 250 nm and 320 nm.The column temperature was set at 30℃and the injection volume was 10μl.Hesperidin was selected as the reference peak.The HPLC fingerprints were analyzed and the similarity was evaluated according to the similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine.Cluster analysis was conducted for the results of content determination by SPSS 22.0 software.Results:The linear range was 4.515-63.210μg·ml^-1 for amygdalin,0.488-6.829μg·ml^-1 for liquiritin,2.288-32.030μg·ml^-1 for hesperidin,0.390-5.461μg·ml^-1 for rosmarinic acid,1.781-24.930μg·ml^-1 for ammonium glycyrrhizinate,1.321-18.490μg·ml^-1 for praeruptorin A and 0.378-5.288μg·ml^-1 for praeruptorin B(r=0.9994-0.9998).The average recovery was 98.6%,98.5%,99.0%,98.7%,99.1%,98.7%and 98.5%(RSD<2.0%,n=6),respectively.Compared with the common pattern of fingerprints,the similarities of 12 batches of samples were greater than 0.9 with 22 common peaks,and 7 of which were identified and assigned.All the 12 batches of samples could be classified into two clusters.Conclusion:The established HPLC fingerprints have a good separation effect and strong characteristics.The method is stable and simple.The better quality control of Xingsu Zhike granules can be achieved by the multi-index composition determination combined with fingerprint analysis.
作者
仲锡铜
耿晖
曹艳花
Zhong Xitong;Geng Hui;Cao Yanhua(Department of Pharmacy,Shandong Provincial Hospital,Ji’nan 250021,China)
出处
《中国药师》
CAS
2020年第10期1935-1940,共6页
China Pharmacist
