安徽农业科学2017，Vol.45Issue(14)：12-13,2.
柱前衍生化-HPLC检测亚氨基二乙酸法制备双甘膦反应进程的研究
Study on the Inspection of the Synthetic Reaction for Preparation of PMIDA with Iminodiacetic Acid by Precolumn Derivatization HPLC
庄勇 1黄楷2
作者信息
- 1. 南通市常海食品添加剂有限公司,江苏海门 226121
- 2. 福建省微生物研究所,福建省新药(微生物)筛选重点实验室,福建福州 350007
- 折叠
摘要
Abstract
[Objective] To establish a new inspection method for preparation of PMIDA with iminodiacetic acid.[Method] The derivatives of the reaction solution for synthesizing PMIDA were synthesized using 9-fluorenyl methyl chloroformate (FMOC-Cl) as the derivatization reagent.The separation of the derivatives was performed on a Gemini C18 column at room temperature by isocratic elution.The mobile phase composed of 60% 0.05 mol/L NaH2PO4 (pH=3.5) and 40% CH3CN at a flow rate of 1.0 mL/min.The injection volume was 10 μL and the detection wavelength was 265 nm.[Result] The linear ranges of the derivatives of iminodiacetonitrile, iminodiacetic acid and ammonia were respectively 0.02-1.20 mg/mL, 0.02-1.20 mg/mL and 0.10-2.00 mg/mL with correlation coefficient of more than or equal to 0.999 8.The detection limits for the derivatives were respectively 0.000 4, 0.000 4 and 0.003 0 mg/mL.The average recoveries of 3 derivatives were respectively 99.96%, 99.86% and 99.89% with relative standard deviation values less than or equal to 1.6%.[Conclusion] The method developed in the present paper could be used for trace analysis of the reaction system for preparation of PMIDA by iminodiacetic acid.关键词
亚氨基二乙酸法/双甘膦/高效液相色谱/衍生化Key words
Iminodiacetic acid/PMIDA/HPLC/Derivatization分类
化学化工引用本文复制引用
庄勇,黄楷..柱前衍生化-HPLC检测亚氨基二乙酸法制备双甘膦反应进程的研究[J].安徽农业科学,2017,45(14):12-13,2.
