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Method for simultaneously detecting betaine hydrochloride and methyl chloroacetate quaternary ammonium salt

A technology of methyl chloroacetate and hydrochloride, applied in the field of analysis of betaine hydrochloride, can solve problems such as no literature reports in the determination, and achieve the effects of prolonging the life of a chromatographic column, reducing errors, and short analysis time

Active Publication Date: 2019-12-13
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no literature report on the determination of methyl chloroacetate quaternary ammonium salt

Method used

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  • Method for simultaneously detecting betaine hydrochloride and methyl chloroacetate quaternary ammonium salt
  • Method for simultaneously detecting betaine hydrochloride and methyl chloroacetate quaternary ammonium salt
  • Method for simultaneously detecting betaine hydrochloride and methyl chloroacetate quaternary ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Shimadzu LC 2030C model high performance liquid chromatography, Anasil AQ-C18 (150mm × 4.6mm, 5μm) chromatographic column.

[0044] Mobile phase: methanol: water (add 2.5mL 40% tetrabutylammonium hydroxide to every 500mL ultrapure water, adjust the pH to 2.00 with phosphoric acid aqueous solution) = 5:95;

[0045] Flow rate: 0.3mL / min;

[0046] Elution mode: isocratic elution;

[0047] Detector: UV detector,

[0048] Detection wavelength: 214nm;

[0049] Column temperature: 30°C;

[0050] Injection volume: 5 μL.

[0051]Weigh 0.5033g of betaine hydrochloride and 0.1109g of refined methyl chloroacetate quaternary ammonium salt, dissolve in mobile phase to 100mL, shake well, filter through a 0.45μm filter membrane, and prepare 5.033mg / mL betaine hydrochloride Salt and 1.109mg / mL methyl chloroacetate quaternary ammonium salt mixed standard solution.

[0052] Weigh 1.5210g of betaine hydrochloride synthesis reaction solution, dissolve it in mobile phase to 100mL, shak...

Embodiment 2

[0057] Shimadzu LC 2030C model high performance liquid chromatography, Anasil AQ-C18 (150mm × 4.6mm, 5μm) chromatographic column.

[0058] Mobile phase: methanol: water (add 2.5mL 40% tetrabutylammonium hydroxide to every 500mL ultrapure water, adjust the pH to 2.40 with phosphoric acid aqueous solution) = 10:90;

[0059] Flow rate: 0.3mL / min;

[0060] Elution mode: isocratic elution;

[0061] Detector: UV detector,

[0062] Detection wavelength: 214nm;

[0063] Column temperature: 40°C;

[0064] Injection volume: 5 μL.

[0065] Weigh 0.5988g of betaine hydrochloride and 0.1227g of refined methyl chloroacetate quaternary ammonium salt, dissolve in mobile phase to 100mL, shake well, filter through a 0.45μm filter membrane, and prepare 5.988mg / mL betaine hydrochloride Salt and 1.227mg / mL methyl chloroacetate quaternary ammonium salt mixed standard solution.

[0066] Weigh 1.9811g of betaine hydrochloride synthesis reaction solution, dissolve it in mobile phase to 100mL, sh...

Embodiment 3

[0071] (1) Preparation of standard solution: Weigh 0.6052g of betaine hydrochloride and 0.1036g of refined methyl chloroacetate quaternary ammonium salt, dissolve it in mobile phase to 100mL, and prepare 6.052mg / mL betaine hydrochloride Salt and 1.036g methyl chloroacetate quaternary ammonium salt prepare betaine hydrochloride and methyl chloroacetate quaternary ammonium salt mixed standard solution.

[0072] (2) Preparation of sample solution: Weigh 1.1564g, 1.0783g, 1.0029g, 1.0924g, 1.1066g, 1.0872g, and 1.0090g of reaction mother liquor, dissolve it in mobile phase and set the volume to 100mL, mix well and filter 0.45μm membrane.

[0073] (3) Determination of standard solution: after the instrument is stabilized, the solution obtained in step (1) is subjected to high performance liquid chromatography determination.

[0074] (4) Determination of sample solution: the solution obtained in step (2) is subjected to high performance liquid chromatography determination.

[0075...

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Abstract

The invention discloses a detection technology for simultaneously analyzing betaine hydrochloride and methyl chloroacetate quaternary ammonium salt in a betaine hydrochloride synthesis reaction liquid. Ion pair chromatography is adopted for separation; an ultraviolet detector is used for detection; a single-point external standard method is used for determining the content of the betaine hydrochloride and the methyl chloroacetate quaternary ammonium salt; and a quality control method is provided for controlling the reaction process of a betaine hydrochloride synthesis process.

Description

technical field [0001] The invention relates to the technical field of analysis of betaine hydrochloride, in particular to a detection technology for simultaneously determining the contents of betaine hydrochloride and methyl chloroacetate quaternary ammonium salt in a reaction solution. Background technique [0002] Betaine hydrochloride is a quaternary ammonium alkaloid. It can not only be used as a high-efficiency methyl donor feed additive to replace choline and methionine in agriculture and animal husbandry, but also has many excellent pharmacological effects. As a surface Active agent has the characteristics of sterilization, synergism, antistatic, anti-hard water, anti-fog, low irritation, thickening, etc. It is widely used in daily chemical, printing and dyeing, petrochemical and other industries. The annual demand is about 100,000 tons. At present, the preparation methods of betaine hydrochloride can be classified into two categories: natural beet molasses extracti...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/34
CPCG01N30/34G01N30/88G01N2030/047G01N2030/884
Inventor 刘启奎岳涛王瑞菲李培培纪晓红张晓霞
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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