Small molecular monocarboxylic acid derivatization-liquid chromatography detection method

A molecular monocarboxylic acid and liquid chromatography technology, applied in the field of organic acid detection, can solve the problems of short analysis time, low detection sensitivity, and affecting the accurate qualitative and quantitative detection of target objects, and achieve the effect of qualitative and quantitative accuracy and high sensitivity

Active Publication Date: 2018-09-21
INST OF SOIL SCI CHINESE ACAD OF SCI +1
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Problems solved by technology

But their main disadvantage is that the complex components in the actual sample will affect the accurate qualitative and quantitative detection of the target object, and it is difficult to detect the low content sample
If a dedicated organic acid determination column is used, the chromatographic column is expensive, and the pretreatment of the sample is complicated, the sample needs to be removed from cations, etc., and there is also the problem of poor detection sensitivity of the instrument; when using the IC method to analyze organic acids, Some organic acids are affected by negative water peaks, making qualitative and quantitative analysis difficult
The CE rule mainly shows that the amount of sample is small, the analysis time is short, and the interference is smaller than that of the HPLC method and the IC method, but the stability of the instrument is worse than that of the HPLC method and the IC method, and there is also detection sensitivity for low-content organic acid samples. The problem is low, and the operating cost is relatively high

Method used

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  • Small molecular monocarboxylic acid derivatization-liquid chromatography detection method
  • Small molecular monocarboxylic acid derivatization-liquid chromatography detection method
  • Small molecular monocarboxylic acid derivatization-liquid chromatography detection method

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Embodiment 1

[0036] 1. Preparation of reagent solution required for derivatization reaction

[0037] 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC) solution: 30-60mmol / L

[0038] 2-(N-morpholino)ethanesulfonic acid (MES) solution: 30-60mmol / L, use NaOH solution to adjust the pH value to 5-6.7

[0039] N-hydroxysuccinimide (NHS) solution: 20-90mmol / L

[0040] Tryptamine solution: 30-60mmol / L, needs to be dissolved with acetone or acetonitrile.

[0041] 2. Standard solution preparation

[0042] Prepare 4 kinds of monocarboxylic acid mixed standard mother liquors: formic acid, acetic acid, propionic acid and butyric acid are all 100mg / L.

[0043] 3. Derivatization reaction

[0044]Derivatization reaction of the standard working curve sample: take an appropriate amount of 4 kinds of monocarboxylic acid mixed standard mother solutions (0-1mL) and add them to a 5mL graduated test tube, and then add an appropriate amount (0.2-1.0mL) of MES solution, 0.1-0.6 mL EDC solution, ...

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Abstract

The invention discloses a small molecular monocarboxylic acid derivatization-liquid chromatography detection method. Chromatographic conditions are as follows: the quantitative detection wavelength is223nm, a chromatographic column is Agilent SB-C18, and the temperature of a column oven is 35 DEG C; acetonitrile and water are used as a mobile phase, and the fixed flow speed is 0.8mL/min; the gradient elution procedure is as follows: the volume ratio of the acetonitrile is 10% at 0 minute, is increased to 70% at 30 minutes and is reduced to 10% at 32 minutes, and the procedure ends at 34 minutes. Several monocarboxylic acid derivatization-liquid chromatography detection methods provided by the invention have qualitative and quantitative accuracy, have the sensitivity which is at least 2 orders of magnitude higher than that in a direct method, can be applied to detection of butyric acid, and have very obvious advantages.

Description

technical field [0001] The invention belongs to an organic acid detection technology in related fields such as agriculture, ecology and environment, and in particular relates to high-sensitivity instrumental analysis and detection of several low-content monocarboxylic acids in ecological environment water samples and plant rhizosphere samples. Background technique [0002] Organic acids widely exist in nature. Small molecule organic acids in the rhizosphere mainly come from the decomposition of animal and plant residues, microbial metabolism, secretion and decomposition of plant roots, and transformation of organic matter applied to the soil. It is a kind of functional organic matter ubiquitous in soil and the most active form of carbon in soil. It can affect the chemical and biological processes of soil through complex mechanisms such as chelation and ligand exchange. The effectiveness of mineral nutrients in the rhizosphere, the mitigation of acidic soil aluminum toxicity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈虹钟明靳伟唐昊冶陈捷俞元春
Owner INST OF SOIL SCI CHINESE ACAD OF SCI
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