摘要
研究了用高效液相色谱法监控以L-谷氨酸为原料,在脱水剂作用下脱水合成L-焦谷氨酸的反应进程。采用YMC-Pack Pro C18反相柱（4.6 mm×250 mm×5μm）,以5 mmol·L-1磷酸二氢钾-0.05 mmol·L-1磷酸二氢铵溶液（用磷酸调p H=3.0）/乙腈（体积比为9∶1）为流动相,通过标准加入法计算反应液中的L-焦谷氨酸含量。结果表明,该监控方法在0.017 8~0.065 3 g·L-1内线性关系良好（相关系数r=0.998 7）;加标平均回收率为99.31%,重复进样的RSD为0.45%。该方法用于实际监控表明,脱水反应可在1 h内完成。
HPLC was applied to monitor the dehydration reaction, in the production process of L - pyroglutamic acid from L - glutamic acid. The chromatography is operated by adopting a YMC - Pack Pro CIS RP column （4.6 mm × 250 mm × 5 μm） and mobile phase composed of aqueous solution of 5 mmol · L-1 potassium dihydro phosphate and 0. 05 mmol ·L-1 ammonium dihydro phosphate in combination of acetonitrile with volume ratio of 9： 1. The content of L - pyroglutamic acid in reaction solution was determined by the standard spiking method. The results showed that the plot of the content and the peak area displays good linearity in the range of 0. 017 8 - 0. 065 3 g · L-1 with r = 0. 998 7; the average recovery is 99.31%, while the relative standard deviation for repetitions is 0. 45%. Based upon this monitoring method ,it showed that the dehydration reaction achieves the best condition at reaction time of 1 h.
出处
《日用化学工业》
CAS
CSCD
北大核心
2014年第11期656-658,共3页
China Surfactant Detergent & Cosmetics
基金
常州市第十七批科技计划(科技支撑-社会发展)资助项目(CE20135011)
