HPLC法同时测定虎杖膏中4种成分的含量

Simultaneous Determination of 4 Components in Reynoutria japonica Cream by HPLC

目的:建立同时测定虎杖膏中虎杖苷、白藜芦醇、大黄素、大黄素甲醚含量的方法。方法:采用高效液相色谱法。色谱柱为Xtimate C_(18),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286 nm,柱温为30℃,进样量为10μL。结果:虎杖苷、白藜芦醇、大黄素和大黄素甲醚检测质量浓度线性范围分别为10~60μg/mL(r=0.999 4)、2.5~15μg/mL(r=0.999 7)、5~30μg/mL(r=0.999 8)、2~12μg/mL(r=0.999 6);定量限分别为0.87、0.44、0.45、0.15μg/mL,检测限分别为0.46、0.15、0.17、0.07μg/mL;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为95.00%~102.00%(RSD=2.25%,n=9)、95.00%~103.00%(RSD=2.97%,n=9)、95.00%~99.56%(RSD=2.05%,n=9)、97.50%~102.50%(RSD=1.59%,n=9)。结论:该方法准确可靠、操作简便,可用于虎杖膏中虎杖苷、白藜芦醇、大黄素、大黄素甲醚含量的同时测定。

OBJECTIVE： To establish a method for the simultaneous determination of polydatin, resveratrol, emodin and phy- scion in Reynoutriajaponica Cream. METHODS： HPLC was performed on the column of Xtimate C18 with mobile phase of acetoni- trile-0.1% Phosphoric acid solution （gradient elution） at a flow rate of 1.0 mL/min, the detection wavelength was 286 nm, column temperature was 30 % ,and the injection volume was 10 μL. RESULTS： The linear range was 10-60 μg/mL for polydatin （r=0.999 4）, 2.5-15 μg/mL for resveratrol （r=0.999 7）, 5-30 μg/mL for emodin （r=0.999 8） and 2-12 ixg/mL for physcion （r=0.999 6）;limit of quantitation was 0.87,0.44,0.45,0.15 μg/mL, limit of detection was 0.46,0.15,0.17,0.07 μg/mL; RSDs of precision, stability and reproducibility tests were lower than 2.0% ;recoveries were 95.00%-102.00% （RSD=2.25% ,n=9）,95.00%-103.00% （RSD= 2.97% , n=9） , 95.00% -99.56% （RSD=2.05% , n=9） and 97.50% -102.50% （RSD=I.59% , n=9） , respectively. CONCLU- SIONS： The method is reliable, simple, and can be used for the simultaneous determination of polydatin, resveratrol, emodin and physcion in R. japonica Cream.