HPLC法测定癌痛消方及其拆方中松脂醇二葡萄糖苷和芍药苷的含量

Determination of Rosinol Diglucoside and Paeoniflorin in Cancer Painkiller and Its Decomposed Formula by HPLC

目的建立癌痛消方及其拆方中松脂醇二葡萄糖苷和芍药苷的测定方法。方法采用十八烷基硅烷键合硅胶柱(Inertsil ODS-3柱250×4.6 mm,5μm);流动相:乙腈-0.1%磷酸(15∶85)为流动相,进行梯度洗脱;检测波长:230 nm(0~16 min,松脂醇二葡萄糖苷),277 nm(16~30 min,芍药苷);流速:1.0 ml/min;柱温:30oC。结果癌痛消-补虚组中松脂醇二葡萄糖苷在1.0~5.0μg范围内呈现良好的线性关系,r=0.9992,平均回收率为97.23%(RSD=1.31%,n=6);癌痛消-抑癌组中芍药苷在1.0~5.0μg范围内呈现良好的线性关系,r=0.9993,平均回收率为97.08%(RSD=1.38%,n=6);癌痛消-全方中松脂醇二葡萄糖苷在1.0~5.0μg范围内呈现良好的线性关系,r=0.9992,平均回收率为98.01%(RSD=1.30%,n=6);癌痛消-全方中芍药苷在1.0~5.0μg范围内呈现良好的线性关系,r=0.9993,平均回收率为96.97%(RSD=1.54%,n=6);结论本方法专属性强,准确度高,重现性良好,可用于癌痛消方的质量控制。

Objective To establish a method for the determination of rosinol diglucoside and paeoniflorin in Cancer Decoction and its decomposed formula.Methods An octadecylsilane bonded silica gel column(Inertsil ODS-3 column 250×4.6 mm,5μm);mobile phase:acetonitrile-0.1%phosphoric acid(15:85)as mobile phase,gradient elution;detection wavelength:230 nm(0~16 min,rosinol diglucoside),277 nm(16~30 min,paeoniflorin);flow rate:1.0 ml/min;column temperature:30oC.Results In the cancer pain-compensation group,rosinol diglucoside showed a good linear relationship in the range of 1.0~5.0μg,r=0.9992,and the average recovery was 97.23%(RSD=1.31%,n=6);The paeoniflorin showed a good linear relationship in the range of 1.0~5.0μg,r=0.9993,and the average recovery was 97.08%(RSD=1.38%,n=6).Cancer pain elimination-total rosin Diglucoside showed a good linear relationship in the range of 1.0~5.0μg,r=0.9992,the average recovery was 98.01%(RSD=1.30%,n=6);The cancer has a good linear relationship in the range of 1.0~5.0μg,r=0.9993,and the average recovery rate is 96.97%(RSD=1.54%,n=6).Conclusion This method has strong specificity.High accuracy and good reproducibility,can be used for quality control of cancer pain.