HPLC波长切换法同时测定苍柏祛痛胶囊中的6种成分

Simultaneous determination of six constituents in Cangbai qutong capsules by HPLC wavelength switching

目的采用HPLC波长切换法同时测定苍柏祛痛胶囊中盐酸黄柏碱、龙胆苦苷、芍药苷、粉防己碱、盐酸小檗碱、丹皮酚等6种成分的含量。方法色谱柱为Waters Xselect CSH-C_(18)柱(150 mm×4. 6 mm,5μm),流动相为乙腈-0. 1%磷酸溶液,梯度洗脱(0～15 min、10%→18%A,15～30 min、18%→50%A,30～35 min、50%→10%A),流速为1. 0 m L·min^(-1),波长为284 nm(0～7 min,盐酸黄柏碱)、274 nm(7～10 min,龙胆苦苷)、230 nm(10～14 min,芍药苷)、274 nm(14～35 min,粉防己碱、盐酸小檗碱、丹皮酚),进样量10μL。结果盐酸黄柏碱、龙胆苦苷、芍药苷、粉防己碱、盐酸小檗碱、丹皮酚进样量分别在0. 150～1. 504、0. 768～7. 680、1. 096～10. 960、0. 220～2. 200、0. 296～2. 956、0. 0345～0. 345μg时与峰面积呈良好的线性关系;平均回收率分别为98. 3%、99. 2%、98. 8%、98. 8%、99. 1%、98. 2%,RSD分别为1. 32%、1. 46%、1. 08%、1. 31%、1. 26%、1. 21%(n=6)。结论所用方法可同时测定制剂中的多种成分,操作简便、准确,重复性好,可用于复方苍柏祛痛胶囊的质量控制。

OBJECTIVE To develop an HPLC wavelength switching method for the simultaneous determination content of 6 components in Cangbai qutong capsules.METHODS The quantitative analysis was carried out on a column of Waters Xselect CSH-C18(150 mm×4.6 mm,5μm),using a mobile phase of acetonitrile(A)-0.1%phosphoric acid(B)by a gradient eluted program(0-15 min,10%→18%A;15-30 min,18%→50%A;30-35 min,50%→10%A)with a flow rate of 1 m L·min-1 at 30℃.The detection wavelength was set at 284 nm(0-7 min,phellodendrine chloride),274 nm(7-10 min,gentiopicroside),230 nm(10-14 min,paeoniflorin),and 274 nm(14-35 min,tetrandrine,berberine hydrochloride,paeonol).RESULTS The linear ranges of phellodendrine chloride,gentiopicroside,paeoniflorin,tetrandrine,berberine hydrochloride and paeonol fell within the ranges of 0.150-1.504μg,0.768-7.680μg,1.096-10.960μg,0.220-2.200μg,0.296-2.956μg and 0.0345-0.345μg,respectively.The recoveries of phellodendrine chloride,gentiopicroside,paeoniflorin,tetrandrine,berberine hydrochloride and paeonol were 98.3%,99.2%,98.8%,98.8%,99.1%and 98.2%,respectively,and the relative standard deviations were 1.32%,1.46%,1.08%,1.31%,1.26%and 1.21%(n=6),respectively.CONCLUSION This method is simple,accurate,reproducible and convenient for the quality control of Cangbai qutong capsules.