【摘要】 提出了用高效液相色谱法监控左旋甲状腺素钠合成关键步骤偶联反应。色谱条件:YMC-Pack Pro C18反相色谱柱(4.6 mm×100 mm5,μm);甲醇-1‰磷酸水溶液为流动相,梯度洗脱;检测波长225 nm;流速1.0 mL/min。偶联反应液在0.05～0.25 mg/mL范围内线性关系良好(相关系数r=0.999 7);加标回收率为99.79%～100.05%;重复进样的平均RSD为1.35%。方法的准确度高,精密度好,实际应用效果好。更多还原

【Abstract】 HPLC was applied to monitor the coupling reaction,which is an important reaction in the synthesis of levothyroxine sodium.Chromatography conditions:YMC-Pack Pro C18 RP column(4.6 mm×100 mm,5 μm);mobile phase:methanol-1‰ phosphoric acid solution by gradient elution;detection wavelength:225 nm;flow rate:1.0 mL/min.The calibration curve was linear in the range of 0.05～0.25 mg/mL of coupling reaction mixture with r=0.999 7;The recovery was 99.79%～100.05% while the relative standard deviation for repetitions was 1.35%.This method has the advantages of quick,correct,reappearing.更多还原