Liquid chromatographic analysis method for simultaneously quantifying glycine and iminodiacetic acid from diethanol amine dehydrogenation product

A technology of iminodiacetic acid and liquid chromatography analysis, applied in the direction of analysis materials, measuring devices, material separation, etc., can solve the problems of toxic derivatization reagents, high derivatization reaction temperature, harsh derivation conditions, etc., and achieve low price and high sensitivity , good stability

Active Publication Date: 2018-01-23
XIANGTAN UNIV
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Problems solved by technology

Such reagents have disadvantages such as high derivatization reaction temperature, harsh derivatization conditions, and toxic derivatization reagents.

Method used

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  • Liquid chromatographic analysis method for simultaneously quantifying glycine and iminodiacetic acid from diethanol amine dehydrogenation product
  • Liquid chromatographic analysis method for simultaneously quantifying glycine and iminodiacetic acid from diethanol amine dehydrogenation product
  • Liquid chromatographic analysis method for simultaneously quantifying glycine and iminodiacetic acid from diethanol amine dehydrogenation product

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Embodiment Construction

[0037] Glycine and iminodiacetic acid have neither chromogenic groups nor fluorescence, but they belong to primary amines and secondary amines respectively, and are prone to Hisberg reaction; after Hisberg reaction with benzenesulfonyl chloride compounds, they are added to the structure of the compound Introducing chromophore groups to achieve detection in liquid chromatography using ultraviolet absorption; the present invention uses p-toluenesulfonyl chloride as a derivatizing agent, and the reaction principle is shown in the following formula:

[0038]

[0039] Compared with other derivatizing agents, p-toluenesulfonyl chloride has the advantages of low price, rapid reaction and few by-products, but it is inevitable that it will also undergo hydrolysis reaction in water; in order to maximize the inhibition of its hydrolysis reaction, the invention adopts a series of optimizations Experiments have found that the optimal reaction conditions are: borax buffer with a temperature of ...

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Abstract

The invention discloses a liquid chromatographic analysis method for simultaneously quantifying glycine and iminodiacetic acid from a diethanol amine dehydrogenation product. The method comprises thefollowing steps: taking toluene sulfonyl chloride acetonitrile as a derivating agent; carrying out derivative reaction on the toluene sulfonyl chloride acetonitrile and amino acid in the diethanol amine dehydrogenation product, and then carrying out liquid chromatographic analysis; and separately drawing standard curves for the concentration of the iminodiacetic acid and the glycine by taking thepeak area of an iminodiacetic acid derivative and the peak area of a glycine derivative. The peak area of an iminodiacetic acid (IDA) standard substance and the concentration of a standard substance have linear dependence in the range of 0.5 g/L-2.500 g/L, the peak area of a glycine (Gly) standard substance and the concentration of a standard substances have linear dependence in the range of 0.01g/L-0.15 g/L, the coefficients of association are greater than 0.9990, and the relative standard deviation is smaller than 1.3%. The analysis result is accurate, analysis steps are simple and convenient, analysis sensitivity is high, the method can be used for quantitative analysis on the iminodiacetic acid as a product and the glycine as a by-product in diethanol amine dehydrogenation reaction, can also be used for liquid chromatography-mass spectrometry qualitative analysis of a product, and has important guidance significance on scientific research and industrial production on preparation of the iminodiacetic acid by diethanol amine catalytic dehydrogenation.

Description

Technical field [0001] The invention relates to a quantitative analysis method capable of simultaneously determining glycine and iminodiacetic acid in diethanolamine dehydrogenation products. Background technique [0002] Iminodiacetic acid (IDA) is an important chemical raw material and an important chemical intermediate with a wide range of uses. It can be used as an intermediate for pesticide oxalylic acid. It can also be used in the electroplating industry, electronics, dyes and water treatment. And many other fields. [0003] At present, the commonly used analytical methods of iminodiacetic acid are: potentiometric titration, ion chromatography, ultraviolet spectrophotometry, gas chromatography pre-column derivatization and reversed-phase high performance liquid chromatography. [0004] (1) Potentiometric titration: Li Yanni. Study on copper zirconium catalyst for the oxidative dehydrogenation of diethanolamine to iminodiacetate. [D]. Zhejiang: Zhejiang Normal University, 2011:...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 段正康张蕾朱宏文尹科徐金霞兰小林
Owner XIANGTAN UNIV
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