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日用化学工业（中英文）

日用化学工业 ›› 2014, Vol. 44 ›› Issue (11): 656-658.doi: 10.13218/j.cnki.csdc.2014.11.146

• 分析与检测 • 上一篇    

高效液相色谱法监控L-焦谷氨酸生产中的脱水反应

叶爱英, 徐瑾, 张文雯, 吴芳珍   

  1. 常州工程职业技术学院 制药与生物工程技术系,江苏 常州 213164
  • 收稿日期:2014-04-24 出版日期:2014-11-22 发布日期:2019-04-08
  • 作者简介:叶爱英(1971-),女,江苏泰兴人,讲师,硕士,电话:13961480063,E-mail:ayye@email.czie.net。
  • 基金资助:
    常州市第十七批科技计划(科技支撑-社会发展)资助项目(CE20135011)

Monitoring of dehydration reaction in the production process of L-pyroglutamic acid by HPLC

YE Ai-ying, XU Jin, ZHANG Wen-wen, WU Fang-zhen   

  1. Department of Pharmaceutics & Biology Engineering and Technology, Changzhou Institute of Engineering Technology,Changzhou,Jiangsu 213164,China
  • Received:2014-04-24 Online:2014-11-22 Published:2019-04-08

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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×5 μm),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pH=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。

关键词: 化妆品原料, L-焦谷氨酸, 脱水反应, 高效液相色谱法

Abstract: 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 C18 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.

Key words: material of cosmetics, L-pyroglutamic acid, dehydration reaction, HPLC

中图分类号: 

  • TQ658