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A kind of preparation and purification method of ion-pair chromatography reagent sodium pentanesulfonate

A technology of sodium pentanesulfonate and ion-pair chromatography, which is applied in the field of preparation and purification of sodium pentanesulfonate, a special reagent for high performance liquid chromatography, can solve the problem of low purity of sodium pentanesulfonate, unsatisfactory separation effect, and dissolution Poor performance and other problems, to achieve the effect of stable and reliable quality, low cost, and short response time

Inactive Publication Date: 2011-12-14
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the sodium pentanesulfonate produced by existing manufacturers has low purity and poor solubility, resulting in unsatisfactory separation effects and failing to achieve the purpose of detection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation and purification method of ion-pair chromatography reagent sodium pentane sulfonate, the specific steps are:

[0023] (2) Sulfonation

[0024] In a 1000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, add 126g of anhydrous sodium sulfite and 450ml of water, then add 98g of bromopentane and 1.6g of tetrapropylammonium bromide, and heat and reflux for 16h until the reaction solution is clear. Layer up.

[0025] (3) Purification

[0026] Under the condition of 82℃ / 20mmHg, the water in the reaction mixture was evaporated under reduced pressure, and the remaining solid was dried, and the mass of the dried solid was 190 g, crush, put into Soxhlet extractor, use 1150 Extract with absolute ethanol to obtain 140 g of crude product, then recrystallize with 2300 ml of absolute ethanol, and obtain pure product after filtration.

[0027] (4) Dry

[0028] The pure product obtained in step (2) is placed in a vacuum drying oven, and 2 g is vacuum...

Embodiment 2

[0030] A preparation and purification method of ion-pair chromatography reagent sodium pentane sulfonate, the specific steps are:

[0031] (1) Sulfonation

[0032] In a 3000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, add 378g of anhydrous sodium sulfite and 1350ml of water, then add 294g of bromopentane and 4g of tetrapropylammonium bromide, heat and reflux for 20h, until the reaction solution is clear and does not separate until.

[0033] (2) Purification

[0034] Under the condition of 82℃ / 20mmHg, the water in the reaction mixture was evaporated under reduced pressure, and the remaining solid was dried to obtain a mass of 550g of dried solid, crushed, put into a Soxhlet extractor, and extracted with 3300ml absolute ethanol to obtain 400g crude product, recrystallized with 6600ml absolute ethanol, and filtered to obtain pure product.

[0035] (3) Drying steps:

[0036] The pure product obtained in step (2) is placed in a vacuum drying oven, and...

Embodiment 3

[0038] A preparation and purification method of ion-pair chromatography reagent sodium pentane sulfonate, the specific steps are:

[0039] (1) Sulfonation

[0040] In a 5000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, add 630g of anhydrous sodium sulfite and 2250ml of water, then add 490g of bromopentane and 5.5g of tetrapropylammonium bromide, and heat and reflux for 24h until the reaction solution is clear. Layer up.

[0041] (2) Purification

[0042] Under the condition of 82℃ / 20mmHg, the water in the reaction mixture was evaporated under reduced pressure, and the remaining solid was dried. The mass of the dried solid was 833g, crushed, put into a Soxhlet extractor, and extracted with 5000ml absolute ethanol. 600g crude product, recrystallized with 10000ml absolute ethanol, and filtered to obtain pure product.

[0043] (3) Dry

[0044] The pure product obtained in step (2) is placed in a vacuum drying oven and vacuum-dried for 4 hours at 80° C...

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Abstract

The invention relates to a preparation and purification method of ion-pair chromatographic reagent sodium pentanesulfonate. The specific steps of the preparation and purification method are: into a reaction vessel, the molar ratio is 1:25:0.65:(0.004~0.006) Add anhydrous sodium sulfite, water, pentane bromide, and tetrapropylammonium bromide in sequence, heat and reflux until the reaction liquid is clear and not stratified; evaporate the water in the reaction liquid under reduced pressure, dry the remaining solid, crush it, and put it into Extract in a Soxhlet extractor, then recrystallize the crude sodium pentanesulfonate obtained from the extraction, filter to obtain the pure product, and then dry it in vacuum to obtain the finished product. In the invention, anhydrous sodium sulfite and bromopentane are subjected to sulfonation reaction under the action of catalyst tetrapropylammonium bromide, and then purified and dried to generate high-quality sodium pentanesulfonate. The method is simple and easy to implement, low in cost and short in reaction time, and the generated sodium pentanesulfonate has good solubility, high purity, product content ≥ 99.6%, stable and reliable quality, and can fully meet the special requirements of high-performance liquid chromatography.

Description

Technical field: [0001] The invention belongs to the field of chromatographic reagents, in particular to a preparation and purification method of sodium pentane sulfonate, a special reagent for high performance liquid chromatography. Background technique: [0002] High-performance liquid chromatograph (HPLC) is widely used in bioengineering, food industry, pharmaceutical industry, petrochemical industry, environment because of its high sensitivity, high resolution, high analysis speed, wide application range and reusable column. Subject areas such as monitoring, commodity inspection, and legal inspection. Ion-pair chromatography reagent sodium pentane sulfonate is an indispensable special reagent for high performance liquid chromatography. It is an aqueous buffer system (mobile phase) composed of phosphate or acetate, and organic modifiers (methanol or acetonitrile). The analytes generated ion pairs are retained on the reversed-phase column to achieve separation. However, the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/04C07C303/44C07C303/32
Inventor 何金
Owner TIANJIN CHEM REAGENT RES INST
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