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Method for measuring organic acid content based on precolumn derivatization LC-MS

A LC-MS, pre-column derivatization technology, applied in the field of analytical chemistry, can solve the problems of the accuracy and sensitivity of detection results need to be improved, and achieve the effect of improving ionization efficiency, high detection sensitivity, and improving detection sensitivity

Inactive Publication Date: 2016-06-22
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can determine various organic acids such as succinic acid, malic acid and citric acid in the cell, and the chromatographic analysis effect is good, but the accuracy and sensitivity of the detection results need to be improved

Method used

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  • Method for measuring organic acid content based on precolumn derivatization LC-MS
  • Method for measuring organic acid content based on precolumn derivatization LC-MS
  • Method for measuring organic acid content based on precolumn derivatization LC-MS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The method for determining the content of citric acid in lemon juice based on LC-MS derivatized before the column may further comprise the steps:

[0033] 1) Preparation of derivatization reagent, sodium carbonate solution and citric acid standard solution

[0034] Accurately weigh 19.9 mg of 2-bromoacetophenone into a dry reagent vial, add 10 mL of anhydrous acetonitrile to prepare a stock solution A with a concentration of 0.01 mol / L, seal it and store it in a refrigerator for later use;

[0035] Accurately weigh 5.3mg of sodium carbonate into a dry reagent vial, add 0.5mL of water to dissolve sodium carbonate, then add 9.5mL of anhydrous acetonitrile to prepare a stock solution B with a concentration of 0.005mol / L, seal it and store it in a refrigerator for later use ;

[0036] Accurately weigh 6.4 mg of citric acid into a dry reagent vial, add 1.5 mL of water to dissolve the citric acid, then add 8.5 mL of anhydrous acetonitrile to prepare a stock solution C with a...

Embodiment 2

[0046] The method for determining malic acid content in apple juice based on pre-column derivatized LC-MS comprises the following steps:

[0047] 1) Preparation of derivatization reagent, sodium carbonate solution and malic acid standard solution

[0048] Accurately weigh 19.9 mg of 2-bromoacetophenone into a dry reagent vial, add 10 mL of anhydrous acetonitrile to prepare a stock solution A with a concentration of 0.01 mol / L, seal it and store it in a refrigerator for later use;

[0049] Accurately weigh 5.3mg of sodium carbonate into a dry reagent vial, add 0.5mL of water to dissolve sodium carbonate, then add 9.5mL of anhydrous acetonitrile to prepare a stock solution B with a concentration of 0.005mol / L, seal it and store it in a refrigerator for later use ;

[0050] Accurately weigh 6.7 mg of malic acid in a dry reagent vial, add 1 mL of water to dissolve the malic acid, then add 9 mL of anhydrous acetonitrile to prepare stock solution C with a concentration of 0.005 mol...

Embodiment 3

[0060] The method for determining the content of citric acid and malic acid in mixed fruit juice based on LC-MS of pre-column derivatization comprises the following steps:

[0061] 1) The preparation of derivatization reagent, sodium carbonate solution, citric acid and malic acid standard solution is the same as in Examples 1 and 2;

[0062] 2) the making of citric acid, malic acid standard curve is also with embodiment 1,2;

[0063] 3) Determination of citric acid and malic acid content in mixed fruit juice

[0064] Derivatization reaction: Take 500 μL of mixed fruit juice in a 50 mL flask, add 500 μL of stock solution A and 500 μL of stock solution B, mix well, and react in an oil bath at 55°C for 24 hours. After the reaction is complete, cool down;

[0065] LC-MS detection: take the reaction product for high performance liquid chromatography-mass spectrometry analysis; the detection conditions of high performance liquid chromatography and mass spectrometry are the same as ...

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Abstract

The invention discloses a method for measuring organic acid content based on precolumn derivatization LC-MS, and belongs to the field of analytical chemistry.The method comprises the steps that 1, a sample to be tested, sodium carbonate and 2-bromoacetophenone are added to a solvent, a derivatization reaction is carried out for 20 h to 28 h at the temperature of 50 DEG C to 60 DEG C after even mixing, and the product is cooled for use; 2, the reaction product in the step 1 is taken for liquid chromatogram-mass spectrum analysis, and the content of organic acid in the sample to be detected is calculated by referring to a standard curve.A chemical modification technology is adopted for derivatization of the organic acid, the physicochemical characteristic of the organic acid is changed, the ionization efficiency can be improved in hygroplasm combined detection, matrix interference can be reduced, meanwhile, interference of inorganic salt and endogenous impurities is reduced, the signal strength ofanalyte is improved, and chromatographic separation and mass spectrometric detection are convenient; then a liquid chromatogram-mass spectrum combined technology is adopted for analyzing and detecting the derivatization product, qualitative and quantitative analysis on the organic acid can be achieved, and the advantages of being simple, efficient, high in detecting sensitivity, good in accuracy and the like are achieved.

Description

technical field [0001] The invention relates to a method for measuring organic acids, in particular to a method for determining the content of organic acids based on pre-column derivatized LC-MS, which belongs to the field of analytical chemistry. Background technique [0002] Organic acids are a class of important substances that affect the flavor of fruits. Their types and contents are closely related to the quality and flavor of fruits and affect the maturity of fruits. They include tartaric acid, malic acid, citric acid, succinic acid, etc., which can improve the body's immunity , Inhibition of brain tissue lipid peroxide generation, anti-cancer and other effects. Accurate analysis and determination of the types and contents of organic acids in samples is of great significance to the research on the types of organic acids in root exudates and the evaluation of fruit flavor characteristics and quality. [0003] At present, the determination methods of organic acids mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/067G01N2030/884
Inventor 卢明华徐林芳王友梅
Owner HENAN UNIVERSITY
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