肾衰宁片的HPLC特征图谱及9个成分的含量测定  

HPLC charateristic chromatograms and determination of nine constituents of Shenshuaining tablets

作　　者：曹舒兴[1] 宋永周[1] 王进[1] CAO Shu-xing;SONG Yong-zhou;WANG Jin(The Second Hospital of Hebei Medical University,Shijiazhuang 050004,China)

机构地区：[1]河北医科大学第二医院,石家庄050004

出　　处：《药物分析杂志》2023年第7期1172-1182,共11页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立肾衰宁片的HPLC特征图谱并测定丹参素、橙皮苷、丹酚酸B、小檗碱、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚这9个成分的含量。方法:采用Agilent Extend C18(250 mm×4.6 mm, 5μm)色谱柱,以乙腈-0.1%磷酸溶液为流动相,进行梯度洗脱,体积流量为1.0 mL·min^(-1),柱温为30℃,检测波长为280 nm;通过相似度评价,结合主成分分析(PCA)和聚类分析(HCA),对10批肾衰宁片的指纹图谱进行分析评价,并对指认的9个成分进行定量测定。结果:建立了肾衰宁片特征指纹图谱,共标定了15个共有峰,各批次样品的相似度均﹥0.99,10批肾衰宁片样品质量存在一定的差异。9个成分分别在各自范围内线性关系良好,平均回收率(n=9)为99.4%~101.1%(RSD在0.49%~1.2%)。10批样品中上述9个成分含量范围依次分别为4.128~4.896、2.684~2.780、8.382~9.806、1.948~2.279、0.327~0.383、0.391~0.457、0.983~1.150、1.191~1.394、0.523~0.612 mg·g^(-1)。结论:建立的肾衰宁片HPLC特征图谱方法及其9个成分含量测定的方法简便、准确、可靠,可用于肾衰宁片的质量评价。Objective:To establish a method for charateristic chromatogram of Shenshuaining tablets and to determine the nine contents of danshensu,hesperidin,salvianolic acid B,berberine,aloe emodin,rhein,emodin,chrysophanol,emodin methyl ether.Methods:Agilent Extend Cis column(250 mm×4.6 mm,5μm)was used,with the mobile phase comprising of acetonitrile-0.1% phosphoric acid solution flowing at 1.0 mL·min^(-1)in a gradient elution manner,the column temperature was 30℃,and the detection wavelength was set at 280 nm.Based on similarity evaluation,principal component analysis(PCA)and hierachical cluster analysis(HCA),the fingerprints of 10 batches of Shenshuaining tablets were analyzed and evaluated,and the 9 components identified were quantitatively determined.Results:The HPLC fingerprint of Shenshuaining tablets was constructed with 15 common chromatographic peaks,the similarities of all batches of samples were all above 0.99 comparing with the reference.There were some differences in the quality of 10 batches of Shenshuaining tablets samples.The linear ranges of nine constituents had good linear relationship within their respective ranges.The average recoveries(n=9)were 99.4%-101.1%with RSDs of 0.49%-1.2%.The content ranges of the above-mentioned nine components in ten batches of samples were 4.128-4.896 mg·g^(-1),2.684-2.780 mg·g^(-1),8.382-9.806 mg·g^(-1),1.948-2.279 mg·g^(-1),0.327-0.383 mg·g^(-1)1,0.391-0.457 mg·g^(-1),0.983-1.150 mg·g^(-1),1.191-1.394 mg·g^(-1),0.523-0.612 mg·g^(-1),respectively.Conclusion:The method of HPLC charateristic chromatograms and the content determination of Shenshuaining tablets is simple,accurate,reliable,and can be used for its quality control.

关 键 词：肾衰宁片 丹参素 橙皮苷 丹酚酸B 小檗碱 芦荟大黄素 大黄酸 大黄素 大黄酚 大黄素甲醚 高效液相色谱 特征图谱 含量测定 质量评价 

分 类 号：R917[医药卫生—药物分析学]