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Liquid chromatography detection method of 3-hydroxypropionaldehyde

A technology of liquid chromatography and detection method, which is applied in the field of liquid chromatography detection of 3-hydroxypropanal, can solve problems such as difficult to achieve chromatographic baseline separation and quantitative detection, and achieve mild derivatization reaction conditions, high sensitivity, and analysis speed fast effect

Pending Publication Date: 2022-05-13
JIANGSU YANGNONG CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the strong polar structure of 3-hydroxypropanal, the 3-hydroxypropanal derivatives and derivatization reagents have the same retention time under common chromatographic conditions, making it difficult to achieve chromatographic baseline separation and quantitative detection

Method used

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  • Liquid chromatography detection method of 3-hydroxypropionaldehyde
  • Liquid chromatography detection method of 3-hydroxypropionaldehyde
  • Liquid chromatography detection method of 3-hydroxypropionaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～4

[0076] Embodiments 1 to 4 provide a liquid chromatography detection method for 3-hydroxypropionaldehyde, the liquid chromatography detection method comprising:

[0077] Mix the acetonitrile solution of 0.20mg / L test sample and dansyl hydrazide, the molar ratio of aldehyde group and dansyl hydrazide in the test sample is 1:4. Then add an acid with a volume percentage of 5%, and conduct a derivatization reaction at 30°C for 60 minutes in an acidic environment to obtain a test solution;

[0078] The liquid to be tested is detected by liquid chromatography under the action of the mobile phase, and the column temperature is 30° C.; the mobile phase includes a combination of the first mobile phase and the second mobile phase; the first mobile phase is acetonitrile, and the The second mobile phase was an aqueous solution containing 0.1 wt% heptafluorobutyric acid ion pair; the flow rate was 1.0 mL / min; the injection volume was 5.0 μL.

[0079] Gradient elution includes:

[0080] Fr...

Embodiment 5～8

[0092] Embodiments 5 to 8 provide a liquid chromatography detection method for 3-hydroxypropionaldehyde. The liquid chromatography detection method all adopts acetic acid, except that the concentration of acetic acid is adjusted, and all the others are the same as in Example 1. The results are shown in the table 2.

[0093] Table 2

[0094] Acid content / % Derivative peak area Example 5 2.0 487 Example 6 3.0 562 Example 7 4.0 566 Example 8 6.0 556

[0095] It can be seen from Table 2 that in the present invention, the acid content is preferably controlled at 3-6%, the peak area of ​​the derivative is more stable, and the test effect is better.

Embodiment 9～13

[0097] Embodiments 9 to 13 provide a liquid chromatography detection method for 3-hydroxypropanal. The liquid chromatography detection methods all adopt acetic acid, and the concentration of acetic acid is 3%. Same as Example 6, the results are shown in Table 3.

[0098] table 3

[0099]

[0100]

[0101] It can be seen from Table 3 that the present invention preferably controls the derivatization time within a specific range, and the peak area of ​​the derivative is more stable and has better test results.

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Abstract

The invention provides a liquid chromatography detection method of 3-hydroxypropionaldehyde, and the liquid chromatography detection method comprises the following steps: carrying out derivatization reaction on a sample to be detected in an acid environment through a derivatization reagent to obtain a liquid to be detected; carrying out liquid chromatography detection on the to-be-detected liquid under the action of a mobile phase; the mobile phase comprises a combination of a first mobile phase and a second mobile phase; the first mobile phase is an organic solvent, and the second mobile phase is an aqueous solution containing heptafluorobutyric acid ion pairs. According to the liquid chromatogram detection method, a derivatization reagent is adopted, a heptafluorobutyric acid ion pair reagent is introduced during liquid chromatogram separation, derivatization reaction conditions are mild, the reaction speed is high, byproducts are few, and the content of trace 3-HPA can be accurately detected.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a liquid chromatography detection method for 3-hydroxypropionaldehyde. Background technique [0002] 3-Hydroxypropionaldehyde (3-HPA) is a three-carbon aldol compound, which is active and easily reacts with mercapto, carboxyl and amino groups. It can be used as a variety of emerging chemicals such as acrolein, acrylic acid and 1 , the precursor of 3-propanediol, etc., used to prepare new polymer materials - poly 1,3-trimethylene terephthalate (PTT), can also be used to produce antifreeze, plasticizer, detergent, preservative and emulsification agent etc. In addition, 3-HPA has a wide range of potential uses in biocidal agents, anti-infection therapeutic agents, bio-crosslinking agents, and precursors of new biomaterials, and is a biochemical raw material with broad application prospects. [0003] 3-HPA is generally produced by hydration of acrolein in industry, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/34G01N30/74
CPCG01N30/06G01N30/34G01N30/74G01N2030/067
Inventor 陶文波张婷丁克鸿徐林黄杰军王根林赵洁徐业庆丁珺王彬陆婷
Owner JIANGSU YANGNONG CHEM GROUP
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