熄风活络胶囊HPLC特征图谱建立及11个成分含量测定

Establishment of HPLC characteristic chromatogram for Xifeng Huoluo capsules and simultaneous determination of eleven constituents

目的:建立熄风活络胶囊的HPLC特征图谱,并测定天麻素、苦杏仁苷、士的宁、羟基红花黄色素A、马钱子碱、芍药苷、阿魏酸、丹酚酸B、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA的含量。方法:熄风活络胶囊的75%甲醇水提取液,采用Venusil MP C18色谱柱(250 mm×4.6 mm, 5μm),以0.1%磷酸水溶液(A)-乙腈(B)作为流动相进行梯度洗脱,体积流量为1.0 mL·min^(-1);柱温为30℃,检测波长为变波长。测定10批熄风活络胶囊特征图谱,标定共有峰并进行归属分析及相似度评价,对采用对照品比对确认的成分进行含量测定。结果:10批熄风活络胶囊特征图谱标定共有峰31个,相似度均大于0.99,归属于12味药材,指认出11个色谱峰。11个成分在各自范围内线性良好(r≥0.999 4),平均加样回收率为99.3%~103.0%,RSD为1.5%~2.4%。结论:所建立的方法灵敏度高,专属性强,HPLC特征图谱结合多成分定量测定能全面地反映其内在质量,可用于熄风活络胶囊的质量控制。

Objective:To establish an HPLC characteristic chromatogram of Xifeng Huoluo capsules,and to determine the contents of gastrodin,amygdalin,strychnine,hydroxysafflower yellow A,brucine,paeoniflorin,ferulic acid,salvianolic acid B,cryptotanshinone,tanshinoneⅠ,and tanshinoneⅡA.Methods:Extraction of 75%methanol was analyzed by a Venusil MP C18 chromatographic column(250 mm×4.6 mm,5μm)using 0.1%phosphoric acid(A)-acetonitrile(B)as the mobile phase with gradient elution at a flow rate of 1.0 mL·min-1.The column temperature was 30℃.The detection wavelengths were variable.The characteristic chromatograms of 10 batches of Xifeng Huoluo capsules were evaluated by similarity evaluation,and the eleven identified index components were quantitatively determined.Results:There were thirty-one common peaks in the characteristic chromatograms of eleven batches of samples and the similarities were all above 0.99.The common peaks could ascribed to twelve medicinal materials,and eleven of them were identified.Eleven components showed good linearity within their respective ranges(r≥0.9994),and the average recoveries were 99.3%-103.0%with RSDs of 1.5%-2.4%.Conclusion:The established method has high sensitivity and strong specificity.The HPLC characteristic chromatogram combined with multi-component quantitative determination can fully reflect its inherent quality and can be used for the quality control of Xifeng Huoluo Capsules.