十枣汤凝胶膏剂HPLC法含量测定研究

Determination of Shizao Decoction Gel Ointment by HPLC

目的研究建立十枣汤凝胶膏剂含量测定方法。方法采用高效液相色谱法,分别以色谱条件Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.8%冰醋酸(65∶35),检测波长338 nm;Neptune C8色谱柱(150 mm×4.6 mm,5μm),流动相为乙腈-0.1%甲酸(86∶14);流速1.0 mL/min,柱温30℃,检测波长210 nm,建立测定十枣汤凝胶膏剂主成分芫花素和大戟二烯醇含量的定量分析方法。结果芫花素在0.09~1.35μg范围呈良好的线性关系,回归方程为Y_(1)=6.221×106X_(1)+2.118×10^(4)(r=0.9998),平均回收率为96.28%(RSD=0.92%),三批凝胶膏剂平均含量分别为0.0692、0.0681、0.0708 mg/g;大戟二烯醇在0.20~4.00μg范围呈良好的线性关系,回归方程为Y_(2)=9.932×10^(5)X_(2)+6.760×10^(4)(r=0.9999),平均回收率为97.69%(RSD=2.37%),三批凝胶膏剂平均含量分别为0.1260、0.1246、0.1276 mg/g。结论建立的十枣汤凝胶膏剂HPLC含量测定法精密度及准确度良好,可用于质量控制。

Objective:To establish a method for determination of Shizao decoction gel ointment.Methods:High-performance liquid chromatography(HPLC)was used to establish a quantitative analysis method to determine the content of genkwanin and euphol in Shizao decoction gel ointment,under the following chromatographic conditions:Diamonsil C18column(250 mm×4.6 mm,5μm)was used with methanol-0.8%glacial acetic(65∶35)as mobile phase,flow rate at 1.0 mL/min,column temperature at 30℃,and detection wavelength at 338 nm;Neptune C8(150 mm×4.6 mm,5μm)was used with acetonitrile-0.1%formic acid(86∶14)as mobile phase,flow rate at 1.0 mL/min,column temperature at 30℃,detection wavelength at 210 nm.Results:The calibration curve was lin-ear within the range of 0.09~1.35μg for genkwanin;the regression equation was Y_(1)=6.221×10~6X_(1)+2.118×10^(4)(r=0.9998);the average recovery was 96.28%(RSD=0.92%);the average content was 0.0692,0.0681 and 0.0708 mg/g.The calibration curve was linear within the range of 0.20~4.00μg for euphol;the regression equation was Y_(2)=9.932×10^(5)X_(2)+6.760×10^(4)(r=0.9999);the average re-covery was 97.69%(RSD=2.37%);the average content was 0.1260,0.1246 and 0.1276 mg/g respectively.Conclusion:The estab-lished HPLC assay method for Shizao decoction gel ointment has good precision and accuracy,which can be used for quality control.