HPLC同时测定保儿安颗粒中5个成分的含量

Simultaneous determination of 5 components in Baoer’an granules by HPLC

目的:建立HPLC法同时测定保儿安颗粒芥子碱硫氰酸酯、夏佛塔苷、牡荆苷、异牡荆苷、山柰酚-3-O-芸香糖苷的含量。方法:采用CAPCEll PAK C_(18)色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.1%磷酸水溶液为流动相进行梯度洗脱,流速为0.8 mL·min^(-1),检测波长为330 nm,柱温为35℃,进样量为10μL。结果:芥子碱硫氰酸酯、夏佛塔苷、牡荆苷、异牡荆苷、山柰酚-3-O-芸香糖苷的线性范围分别为0.40~12.64μg·mL^(-1)(r=1.000)、0.33~10.57μg·mL^(-1)(r=0.9998)、0.47~15.01μg·mL^(-1)(r=0.9997)、0.16~5.06μg·mL^(-1)(r=0.9998)、0.27~8.50μg·mL^(-1)(r=0.9990);平均回收率(n=3)范围分别为100.9%~102.2%、96.5%~97.3%、96.2%~97.0%、95.6%~99.1%、99.0%~100.2%;14批保儿安颗粒中上述5个成分含量分别为11.05~40.90、10.64~37.75、14.29~63.77、6.73~26.57、7.43~35.23μg·g^(-1)。14批样品聚类分为4类。结论:所建方法简便,稳定可行,重复性好,可用于保儿安颗粒的质量控制和评价。

Objective:To establish an HPLC method for the simultaneous determination of sinapine thiocyanate,schaftoside,vitexin,isovitexin and kaempferol-3-O-rutinoside in Baoer’an granules.Methods:CAPCEll PAK C_(18)(250 mm×4.6 mm,5μm)column was used with methanol-0.1%phosphoric acid solution as mobile phase in gradient elution at a flow rate of 0.8 mL·min^(-1),and the detection wavelength was 330 nm,the column temperature was 35℃and the injection volume was 10μL.Results:The linear ranges of sinapine thiocyanate,schaftoside,vitexin,isovitexin and kaempferol-3-O-rutinoside were 0.40-12.64μg·mL^(-1)(r=1.000),0.33-10.57μg·mL^(-1)(r=0.9998),0.47-15.01μg·mL^(-1)(r=0.9997),0.16-5.06μg·mL^(-1)(r=0.9998)and 0.27-8.50μg·mL^(-1)(r=0.9990),respectively.The average recoveries(n=3)were 100.9%-102.2%、96.5%-97.3%、96.2%-97.0%、95.6%-99.1%and 99.0%-100.2%,respectively.The contents for sinapine thiocyanate,schaftoside,vitexin,isovitexin and kaempferol-3-O-rutinoside in 14 batches of Baoer’an granules were 11.05-40.90,10.64-37.75,14.29-63.77,6.73-26.57 and 7.43-35.23μg·g^(-1).The samples of 14 batches of Baoer’an granules could be divided into 4 categories.Conclusion:The method developed is simple,stable and repeatable,which can be used for the quality control of Baoer’an granules.