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Purification method of methanol for liquid chromatography-mass spectrometry

A technology of liquid chromatography and purification method, which is applied in the field of methanol purification for liquid chromatography-mass spectrometry, which can solve problems such as misjudgment, difficulty in purification, and reduction of the accuracy of liquid chromatography measurement results, and expand the scope of application , low energy consumption, and the effect of reducing the cost of imports

Active Publication Date: 2018-01-16
上海星可高纯溶剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a mobile phase solvent, the higher the purity, the better the separation effect of organic matter in the sample, and the high-purity solvent can avoid the phenomenon of insufficient ionization of the analyte caused by the existence of impurities, especially metal ions. In the mass spectrometry analysis, it complexes with the measured substance and produces interference peaks in the mass spectrometer, which leads to misjudgment of the determination of molecular weight and other parameters, and greatly reduces the accuracy of the liquid chromatography-mass spectrometry measurement results
[0004] As a solvent with excellent performance, methanol can dissolve various organic, inorganic and gaseous substances, but its purification is very difficult

Method used

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  • Purification method of methanol for liquid chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The method for purifying methanol for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0024] a. Take the raw material methanol, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide, etc. Impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 8. After the oxidation treatment, methanol is rapidly distilled off.

[0025] a'. Will add reducing agent ferrous oxide and stir in the methanol obtained in step a, distill out methanol.

[0026] b. Add sodium carbonate to the distilled methanol to adjust the pH of the solution to 7, and shake to make the sodium carbonate fully react with the acidic impurities in the ra...

Embodiment 2

[0033] The method for purifying methanol for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0034] a. Take the raw material methanol, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide, etc. Impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 14. After the oxidation treatment, methanol is rapidly distilled off.

[0035] a'. Add reducing agent sodium bisulfate to the methanol obtained in step a and stir to distill out methanol.

[0036] b. Add potassium hydroxide to the above-mentioned distilled methanol to adjust the pH of the solution to 8, and shake to make the potassium hydroxide fully react with the acid...

Embodiment 3

[0043] The method for purifying methanol for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:

[0044] a. Take the raw material methanol, add potassium permanganate to it for oxidation treatment, remove impurities containing double bonds such as ethylene, acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide, etc. Impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 10. After the oxidation treatment, methanol is rapidly distilled off.

[0045] a'. Add reducing agent disodium hydrogen phosphate to the methanol obtained in step a and stir to distill out methanol.

[0046] b. Add sodium oxide to the above-mentioned distilled methanol to adjust the pH of the solution to 7.5, and shake to make the sodium oxide fully react with the acidi...

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Abstract

The invention discloses a method for purifying methanol for liquid chromatography-mass spectrometry, which is characterized in that impurities in raw methanol are removed through processes such as modified activated carbon adsorption to obtain methanol for liquid chromatography-mass spectrometry . The method for purifying methanol used in liquid chromatography-mass spectrometry provided by the invention can obtain methanol with a purity ≥ 99.99% (wt), which meets the high-purity requirements of liquid chromatography-mass spectrometry, so that the purified methanol can It is applied to the field of liquid chromatography-mass spectrometry, expanding the scope of application.

Description

technical field [0001] The invention relates to the field of solvent purification, in particular to a method for purifying methanol used in liquid chromatography-mass spectrometry. Background technique [0002] The online coupling of chromatography-mass spectrometry combines the separation ability of chromatography with the qualitative function of mass spectrometry to achieve more accurate quantitative and qualitative analysis of complex mixtures. It also simplifies the pretreatment process of the sample and makes the sample analysis easier. Chromatography-mass spectrometry includes gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry. Liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry complement each other to analyze compounds of different properties. [0003] Liquid Chromatograph Mass Spectrometer (LC-MS for short) is a high-end instrument in the organic analysis market. Liquid chromatography (LC) can effectively ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/04C07C29/74C07C29/76C07C29/92
Inventor 范文林张群星张怡魏丽
Owner 上海星可高纯溶剂有限公司
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