HPLC-ELSD 测定蛇胆川贝散生产过程西贝母碱的含量变化

目的: 检测蛇胆川贝散生产过程中西贝母碱含量的变化,为生产工艺和质量控制提供实验依据。方法: 用Agilent TC-C₁₈ (4.6 mm×250 mm, 5 μm)色谱柱,以乙腈- 0.02%二乙胺水溶液系统为流动相,流速1.0 mL ·min^-1;蒸发光散射检测器的漂移管温度40 ℃,气体流速2.4 L ·min^-1,增益1。结果: 西贝母碱在进样量1.032~20.64 μg与峰面积呈良好线性关系(r=0.999 97), 方法回收率为98.90% (RSD为2.89%)。蛇胆川贝散原料药灭菌前后及制剂成品中含量分别为0.333 6,0.318 6,0.293 0 mg ·g^-1。结论: 本方法快速、简便、准确、重复性好, 能快速准确测定制剂过程中的原料药、灭菌后中间品和制剂成品的含量,为本品质量控制提供依据。

Determination of Sipeimine in Shedan Chuanbei Powder by HPLC-ELSD

Objective: To establish a HPLC-ELSD method for the determination of sipeimine in shedan chuanbei powder of different process of production.Method: The column of TC-C18(4.6 mm×250 mm,5 μm) was used.The mobile phase was acetonitrile-0.06% diethylamine-water.Drift tube temperature of ELSD was 40 ℃,gas flow was 2.4 L·min-1 and gain was 1.Result: The sipeimine calibration curves were linear in the range of 1.032-20.64 μg,r=0.999 97).The average recovery was 98.90% with the RSD value of 2.89%(n=6).Sipeimine of the sample in Shedan Chuanbei Powder production process were 0.333 6,0.318 6,0.293 0 mg·g-1.Conclusion:The method can be used to determine the content of sipeimine in Shedan Chuanbei powder.