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Preparation method of ion-pair chromatographic-grade tetradecyl trimethyl ammonium bromide

A technology of tetradecyltrimethylammonium bromide and ion-pair chromatography, which is applied in the field of analytical chemistry, can solve problems such as the inability to meet the technical requirements for ion-pair chromatography analysis, achieve simple operation, reduce product costs, and have obvious economic benefits Effect

Inactive Publication Date: 2019-05-24
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, even if the content of tetradecyltrimethylammonium bromide in the market reaches analytical purity, there are still traces of impurities with high ultraviolet absorption, which cannot meet the technical requirements of ion-pair chromatography analysis.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation technology of ion-pair chromatographic grade tetradecyltrimethylammonium bromide, the steps are as follows:

[0022] Put 180g of tetradecyltrimethylammonium bromide raw material into 720mL of solvent (the solvent is prepared from 540mL of anhydrous acetone and 180mL of anhydrous methanol); Heating, adding in batches 9g particle diameter 100 orders through pretreated activated carbon (the mass concentration of activated carbon is the hydrogen peroxide soaking 8h of 30%) in the gained solution under stirring, soaks 5h with 6N nitric acid solution after separation, solid-liquid separation, uses Wash with ionic water until neutral, vacuum dry at 100°C for 4h, and vacuum degree is 0.001MPa), then heat to reflux and fully stir for 3h, stop heating, filter under reduced pressure, cool the filtrate to room temperature, transfer to a crystallizer, stand and separate The crystallization temperature is -20°C; the separated white crystals are separated by filt...

Embodiment 2

[0029] A kind of preparation technology of ion-pair chromatographic grade tetradecyltrimethylammonium bromide, the steps are as follows:

[0030] Put 400g of tetradecyltrimethylammonium bromide raw material into 800mL of solvent (the solvent is prepared from 400mL of anhydrous acetone and 400mL of anhydrous methanol); the resulting mixture is heated to 60°C and stirred for not less than 1h, Stop heating, add 27g particle diameter 400 mesh pretreated activated carbons in batches under stirring (the activated carbons are soaked in 30% hydrogen peroxide for 12 hours, soaked in 6N nitric acid solution for 8 hours after separation, separated from solid and liquid, used Wash with ionic water until neutral, vacuum dry at 100°C for 6h, vacuum degree is 0.001MPa); heat to reflux and fully stir for 8h, stop heating, filter under reduced pressure, cool the filtrate to room temperature, transfer to a crystallizer, stand still and crystallize, The crystallization temperature is -10°C; filt...

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Abstract

The invention discloses a preparation method of ion-pair chromatographic-grade tetradecyl trimethyl ammonium bromide. The preparation technology is characterized by comprising the steps that a tetradecyl trimethyl ammonium bromide raw material is put into a solvent, heating is conducted to 55-60 DEG C, stirring is conducted for 1h or longer, and heating is stopped; under the stirring condition, pretreated activated carbon is added to the obtained solution in batch, heating reflux is conducted, sufficient stirring is conducted for 3-8 h, heating is stopped, pressure reduction and suction filtration are conducted, a filtrate is cooled to the room temperature and transferred to a crystallizer, and standing and crystallization are conducted; separated white crystals are filtered and separated,a filter cake is press-dried, the crystals are collected, drying is conducted, and the ion-pair chromatographic-grade tetradecyl trimethyl ammonium bromide is obtained and subjected to sealing packaging under nitrogen protection. The method is easy, convenient and quick to operate and efficient.

Description

technical field [0001] The invention relates to a special reagent for high-performance liquid chromatography analysis, in particular to a preparation process of ion-pair chromatography grade tetradecyltrimethylammonium bromide, which belongs to the technical field of analytical chemistry. Background technique [0002] Ion pair chromatography (IPC) is to add ions (paired ions or counter ions) with opposite charges to the analyzed ions into the mobile phase, and combine with solute ions to form weakly polar ion pairs. It is a chromatographic mode in which the phase is not easy to dissociate and quickly transfers to the bonded phase, and then distributes between the stationary phase and the mobile phase, and finally achieves separation. Due to the addition of ion-pair reagents, ion-pair chromatography has the advantages of simple operation and high separation column efficiency in the determination of ionic compounds, and is widely used in the fields of medicine, biochemistry, d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/84
Inventor 程俊徐久振姜苏凌青
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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