High performance liquid chromatography analysis method for oxalic aldehyde and glyoxalic acid

A high-performance liquid chromatography, glyoxal technology, applied in the direction of analysis of materials, material separation, measurement devices, etc., can solve the problems of time-consuming detection, easy to interfere with results, difficult to quantify, etc., to achieve a high degree of automation, tedious compensation process, Detect sensitive effects

Inactive Publication Date: 2009-08-19
NANJING UNIV OF TECH
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Problems solved by technology

However, regarding the quantitative detection of the products and by-products of glyoxal produced by the acetaldehyde oxidation method, the industry has always used traditional chemical analysis and determination, which has many procedures and is time-consuming. The qualitative and quantitative determination of each product in the reaction process The instrumental analysis method has not been solved yet, and the research on the analysis method of glyoxal and glyoxylic acid in the acetaldehyde solution has not yet been reported
[0004] In recent years, some scholars have studied the analysis of glyoxal and glyoxylic acid, such as Hu Jun et al. University Journal, 2001, 27 (1): 34-37) adopt Cannizzaro reaction to measure glyoxal content in the electrolytic solution of glyoxylic acid by anodic oxidation of glyoxal, aldehyde total amount is measured with sodium sulfite method, acetaldehyde The quantification of acid subtracts the amount of glyoxal from the total amount of aldehydes, which is time-consum...

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  • High performance liquid chromatography analysis method for oxalic aldehyde and glyoxalic acid
  • High performance liquid chromatography analysis method for oxalic aldehyde and glyoxalic acid
  • High performance liquid chromatography analysis method for oxalic aldehyde and glyoxalic acid

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Embodiment 1

[0043] A. Drawing of glyoxal standard curve

[0044]a), preparation of glyoxal standard solution: take 1mL of 40wt% glyoxal solution, in a 50mL volumetric flask, use deionized water to constant volume to obtain a 10g / L glyoxal solution, pipette 1mL in a 100mL volumetric flask To get 0.1g / L glyoxal solution, pipette 1, 1.5, 2.5, 3.5, 5, 10mL respectively into 50mL volumetric flask, and make 0.002, 0.003, 0.005, 0.007, 0.01, 0.02g / L glyoxal Aldehyde standard sample solution;

[0045] b) Preparation of glyoxal-DNPH derivative samples: take 0.002, 0.003, 0.005, 0.007, 0.01, 0.02g / L glyoxal standard sample solution 1mL respectively, add 10mL0.2g / LDNPH solution (dissolved in acetonitrile) , using 5% phosphoric acid solution to adjust the pH to 2, reacting in a constant temperature water bath at 60°C for 120 minutes to obtain glyoxal-DNPH derivatives with different concentrations;

[0046] c) Agilent 1100 high-performance liquid chromatograph is used as an analyzer, equipped with a...

Embodiment 2

[0055] Use this method to detect the mixed reaction product solution of glyoxal by oxidation of acetaldehyde: dilute the reaction solution 10000 times, take 1mL diluted sample, add 10mL 0.2g / LDNPH solution (dissolved in acetonitrile), and adjust the pH with 5% phosphoric acid solution After reaching 2, react for 120 minutes in a constant temperature water bath at 60°C. The result is as Figure 4 shown. The abscissa in the figure is the retention time / min, and the ordinate is the absorbance / mAU. From Figure 4 It can be seen that two peaks a and b appear at the corresponding retention times of DNPH and glyoxal dihydrazone, and the separation of the peaks is very good. In addition, there are no other peaks, indicating that the content of glyoxylic acid and acetaldehyde is very low, even lower than the detection limit, and the by-products acetic acid and oxalic acid do not interfere with the detection of glyoxal dihydrazone. Substitute the peak area of ​​glyoxal dihydrazone i...

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Abstract

The invention relates to a high-performance liquid chromatography (HPLC) analytical method of glyoxal and glyoxylate comprising the following specific detection steps of: taking proper amount of samples; adding DNPH, the mole ratio of which to the aldehyde group is 2:1 to 50:1, as a derivative reagent; adjusting the pH to 1.5 to 3 by using weak-acid salt solution; reacting in thermostatic water bath at 30 to 80 DEG C for 60 to 240 minutes; and analyzing the obtained derivative by using HPLC with the ultraviolet detection wavelength of 400-500 nm. The HPLC analysis conditions are as follows: the mobile phase is acetonitrile and aqueous solution, with the volume ratio of 95/5 to 50/50; the flow rate is 0.6 to 2ml/min; the column temperature is 20 to 50 DEG C; and the sample size is 1 to 20 Mu L. The HPLC analytical method of glyoxal and glyoxylate has the advantages of high degree of automation, high selectivity, sensitive detection, high efficiency and accuracy and the like. Experimental results show that the acetaldehyde, acetic acid and oxalic acid can not generate mutual interference to the detection of the glyoxal and glyoxylate.

Description

technical field [0001] The invention relates to an analysis method of glyoxal and glyoxylic acid, in particular to a high performance liquid chromatography analysis method using 2,4-dinitrophenylhydrazine (DNPH) to derive glyoxal and glyoxylic acid. The invention belongs to the technical field of chemical analysis and instrumental analysis in the chemical industry. Background technique [0002] Glyoxal, also known as oxalic acid aldehyde, is the simplest α-dicarbonyl compound. In addition to the generality of aliphatic aldehydes, it also has some special chemical properties. It can be combined with alcohols, amines, amides, aldehydes and hydroxyl-containing It can also undergo addition or condensation reaction with protein-like animal glue, cellulose, polyvinyl alcohol and urea, etc. It is a widely used chemical raw material and intermediate, used in papermaking, textile printing and dyeing , coatings, medicine, building materials, petrochemical, environmental protection an...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 王海燕崔群朱鸭梅
Owner NANJING UNIV OF TECH
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