HPLC法同时测定龙泽熊胆胶囊中6种成分的含量

摘要

OBJECTIVE:To establish a method for simultaneous determination of chlorogenic acid,geniposide,gentiopicro-side,baicalin,berberine hydrochloride and chrysophanol in Longze xiongdan capsule. METHODS:HPLC method was adopted. The separation was performed on Dikma Platisil ODS column with mobile phase consisting of acetonitrile-0.1% phosphoric acid so-lution(gradient elution)at the flow rate of 1.0 mL/min. The detection wavelength were set at 254 nm for geniposide,gentiopicro-side,baicalin,berberine hydrochloride and chrysophanol and 327 nm for chlorogenic acid. The column temperature was 30 ℃. RE-SUITS:Linear ranges of chlorogenic acid,geniposide,gentiopicroside,baicalin,berberine hydrochloride and chrysophanol were 0.0082-0.164 μg (r=0.9998),0.027-0.540 μg(r=0.9997),0.02525-0.505 μg(r=0.9998),0.046-0.920 μg(r=0.9997), 0.059-1.180 μg(r=0.9995),0.00805-0.161 μg(r=0.9994),respectively;the limits of quantitation were 0.61,0.59,0.87,0.51, 0.92,0.65 ng,and the limits of detection were 1.67,1.73,1.96,1.82,2.31,1.87 ng. RSDs of precision,stability and reproduc-ibility tests were lower than 2.0%;recoveries were 95.34%-98.27%(RSD=1.2%,n=9),98.18%-101.92%(RSD=1.4%,n=9), 97.36% -101.09%(RSD=1.0% ,n=9),95.24% -98.93%(RSD=1.3% ,n=9), 95.76% -99.34%(RSD=1.5% ,n=9), 95.00%-98.75%(RSD=1.4%,n=9),respectively. CONCLUSIONS:The method is simple,accurate,reproducible and suitable for simultaneous determination of chlorogenic acid,geniposide,gentiopicroside,baicalin,berberine hydrochloride,chrysophanol in Longze xiongdan capsule.%目的:建立同时测定龙泽熊胆胶囊中绿原酸、栀子苷、龙胆苦苷、黄芩苷、盐酸小檗碱、大黄酚6种成分含量的方法.方法:采用高效液相色谱法.色谱柱为Dikma Platisil ODS,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm(栀子苷、龙胆苦苷、黄芩苷、盐酸小檗碱、大黄酚)、327 nm(绿原酸),柱温为30℃.结果:绿原酸、栀子苷、龙胆苦苷、黄芩苷、盐酸小檗碱、大黄酚检测进样量线性范围分别为0.0082~0.164μg(r=0.9998)、0.027~0.540μg(r=0.9997)、0.02525~0.505μg(r=0.9998)、0.046~0.920μg(r=0.9997)、0.059~1.180μg(r=0.9995)、0.00805~0.161μg(r=0.9994);定量限分别为0.61、0.59、0.87、0.51、0.92、0.65 ng,检测限分别为1.67、1.73、1.96、1.82、2.31、1.87 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为95.34%~98.27%(RSD=1.2%,n=9)、98.18%~101.92%(RSD=1.4%,n=9)、97.36%~101.09%(RSD=1.0%,n=9)、95.24%~98.93%(RSD=1.3%,n=9)、95.76%~99.34%(RSD=1.5%,n=9)、95.00%~98.75%(RSD=1.4%,n=9).结论:该方法操作简便、结果准确、重复性好,可用于龙泽熊胆胶囊中绿原酸、栀子苷、龙胆苦苷、黄芩苷、盐酸小檗碱、大黄酚含量的同时测定.