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研究了用HPLC法监控L-噻唑烷-4-甲酸乙酯合成关键步骤酯化反应。色谱条件:YMC-Pack Pro C18反相柱(4.6 mm×150 mm×5μm);0.01 mol/L磷酸二氢钠溶液(用磷酸调节pH为2.0)-甲醇为流动相,检测波长210 nm;流速1.0 mL/min。酯化反应液在0.158~1.278 mg/mL范围内线性关系良好(相关系数r=0.997 6);加标平均回收率为94.70%,重复进样的RSD为0.08%~1.62%,该方法的准确度高,精密度好,实际监测效果好。
The key step of esterification of ethyl L-thiazolidine-4-carboxylate was monitored by HPLC. Chromatographic conditions: YMC-Pack Pro C18 reversed-phase column (4.6 mm × 150 mm × 5 μm); 0.01 mol / L sodium dihydrogen phosphate solution (adjusted to pH 2.0 with phosphoric acid) -Methanol as the mobile phase at a detection wavelength of 210 nm; 1.0 mL / min. The linearity of the esterification reaction was good in the range of 0.158-1.278 mg / mL (correlation coefficient r = 0.997 6). The average recovery was 94.70% and the RSD of repeated injection was 0.08% -1.62% High degree, good precision, the actual monitoring effect is good.