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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0.008 2~0.164 μg (r=0.999 8)、0.027~0.540 μg(r=0.999 7)、0.025 25~0.505 μg(r=0.999 8)、0.046~0.920 μg(r=0.999 7)、0.059~1.180 μg(r=0.999 5)、0.008 05~0.161 μg(r=0.999 4);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。
OBJECTIVE: To establish a method for simultaneous determination of chlorogenic acid, geniposide, gentiopicroside, 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 solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength were set at 254 nm for geniposide, gentiopicroside, baicalin, berberine hydrochloride and chrysophanol and 327 nm for chlorogenic acid. The column temperature was 30 ℃. RESUITS: Linear ranges of chlorogenic acid, geniposide, gentiopicroside, baicalin, berberine hydrochloride and chrysophanol were 0.008 2-0.164 μg (r=0.999 8),0.027-0.540 μg(r=0.999 7),0.025 25-0.505 μg(r=0.999 8),0.046-0.920 μg(r=0.999 7),0.059-1.180 μg(r=0.999 5),0.008 05-0.161 μg(r=0.999 4), 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 reproducibility 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.
高效液相色谱法龙泽熊胆胶囊绿原酸栀子苷龙胆苦苷黄芩苷盐酸小檗碱大黄酚含量
HPLCLongze xiongdan capsuleChlorogenic acidGeniposideGentiopicrosideBaicalinBerberine hydrochlorideChrysophanolContent
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