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

作　　者：庄勇 黄楷[2] 

机构地区：[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

出　　处：《安徽农业科学》2017年第14期12-13,共2页Journal of Anhui Agricultural Sciences

摘　　要：[目的]建立一种利用亚氨基二乙酸制备双甘膦的新检测方法。[方法]以9-芴基甲氧羰酰氯为衍生化试剂对合成双甘膦的反应物进行衍生化。采用Gemini C_(18)(150.0 mm×4.6 mm,5.0μm)色谱柱,室温下以0.05 mol/L NaH_2PO_4(pH=3.5)溶液-乙腈(V/V,60∶40)为流动相,流速为1.0 m L/min,检测波长265 nm,对反应液中的亚氨基二乙腈、亚氨基二乙酸和氨气衍生物进行分离检测。[结果]反应液中的亚氨基二乙腈、亚氨基二乙酸和氨气衍生物,分别在0.02~1.20、0.02~1.20、0.10~2.00 mg/m L浓度范围内呈现良好的线性关系(r≥0.999 8),检出限分别为0.000 4、0.000 4、0.003 0 mg/m L,加样回收率分别为99.96%、99.86%、99.89%,相对标准偏差均不超过1.6%。[结论]该研究建立的方法可用于亚氨基二乙酸法制备双甘膦反应体系的跟踪分析。[ 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-C1） 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 NaHzPO4 （ pH = 3.5 ） and 40% CH3 CN at a flow rate of 1.0 mL/min. The injection volume was 10μL 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 

分 类 号：O657.7[理学—分析化学]