蜘蛛香胶囊中橙皮苷的TLC鉴别和HPLC测定

TLC Identification and HPLC Determination of Hesperidin in Valeriana Jatamansi Capsule

旨在建立蜘蛛香胶囊中橙皮苷的薄层色谱(TLC)鉴别和高效液相色谱(HPLC)含量测定的方法。采用TLC法对橙皮苷进行定性鉴别,以乙酸乙酯-甲醇-水(100∶17∶13)为展开剂,三氯化铝试液为显色剂;采用HPLC法测定制剂中橙皮苷含量,使用C18色谱柱(4.6×250mm,5μm),流动相为甲醇-冰醋酸-水(35∶4∶61),流速1.0mL/min,检测波长284nm,柱温30℃,进样量20μL。结果显示,TLC法操作简便,斑点清晰,专属性强,能鉴别出橙皮苷;HPLC方法中,橙皮苷在0.16～6.4μg范围内与峰面积呈良好线性关系(r=0.9999),平均回收率为97.7%(n=6),RSD为1.3%,6批次蜘蛛香胶囊中的橙皮苷平均含量为2.08mg/粒。结果表明,所建立的TLC法能鉴别橙皮苷,HPLC法能准确测定橙皮苷含量,为蜘蛛香胶囊的质量控制提供了科学依据。

The experiment was aimed to establish a method for identification and determination of hesperidin in Valeriana jatamansi capsule by thin-layer chromatography(TLC)and high performance liquid chromatography(HPLC).Hesperidin was identified by TLC,using ethyl acetate-methanol-water(100∶17∶13)as the mobile phase and alchlor solution as the chromogenic agent.The content of hesperidin was detected by HPLC.The separation was carried out on a CAPCELL PAK C18MG column(4.6×250mm,5μm)with the mobile phase of methanol-glacial acetic acid-water(35∶4∶61)at the flow rate of1.0mL/min,the detection wavelength was284nm,the column temperature was30℃,and the injection volume was20μL.Hesperidin could be identified by TLC,and TLC method was simple and the spots were clear and strongly specific.The linear range of hesperidin was0.16-64μg(r=0.9999),the average recovery rate was97.7%,and RSD was1.3%(n=6).The average content of hesperidin in each Valeriana jatamansi capsule was2.08mg from6batches.The results suggested that hesperidin could be identified by TLC and determined by HPLC,and the established method could be used for the quality control of Valeriana jatamansi capsule.