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

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...

AI Technical Summary

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-consuming, susceptible to interference and large error in results; Xu Jialiang et al. Research. Analytical Laboratory, 1998, 17 (5): 41-44) reported the use of UV spectrophotometry to measure the content of glyoxal, and achieved certain results, but the UV spectrophotometry is not intuitive enough and susceptible to interference; Shigehisa Uchiyama et al. (Shigehisa Uchiyama, Erika Matsushima, Hiroshi Tokunaga, et. al. Determination of orthophthalaldehyde in air using 2,4-dinitrophenylhydrazine-impregnated silicacartridge and high-performance liquid chromatography. Journal of Chromatography A, 2006, (16116) ) reported the method of using 2,4-dinitrophenylhydrazine as a derivative reagent to detect phthalaldehyde in the air, but in this method, phthalaldehyde reacted with 2,4-dinitrophenylhydrazine to generate phthalaldehyde Aldehyde monohydrazone and o-phthalaldehyde dihydrazone, but not all generate o-phthalaldehyde dihydrazone, and the two are easy to transform into each other, so it is not easy to quantify

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