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Preparation method for ion-pair chromatography reagent sodium heptanesulfonate

A technology of sodium heptane sulfonate and ion-pair chromatography is applied in the preparation of sulfonates, the preparation of organic compounds, chemical instruments and methods, etc. To detection and other issues, to achieve the effect of stable and reliable quality, low cost and reduced usage

Inactive Publication Date: 2012-05-02
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 heptanesulfonate 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

[0019] A preparation and purification method of ion-pair chromatography reagent sodium heptanesulfonate, comprising the following steps:

[0020] (1) Sulfonation: Add 126 grams of anhydrous sodium sulfite and 450 ml of water into a 1000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, then add 125 grams of bromoheptane and 1.2 grams of tetrapropylammonium bromide, and heat to reflux 16 hours until the reaction solution was clear and separated.

[0021] (2) Purification: steam the moisture in the reaction mixture under reduced pressure at 82° C. / 20 mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 1300 ml of absolute ethanol to obtain 162 grams of crude product. Then use 2600ml of absolute ethanol to recrystallize, and obtain the pure product after filtration.

[0022] (3) Drying: the purified product was placed in a vacuum oven and dried for 2 hours at 80° C. / 100 mmHg to obtain 132 grams of fin...

Embodiment 2

[0024] A preparation and purification method of ion-pair chromatography reagent sodium heptanesulfonate, comprising the following steps:

[0025] (1) Sulfonation: In a 5000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, add 378g of anhydrous sodium sulfite and 1350ml of water, then add 376g of bromoheptane and 5g of tetrapropylammonium bromide, and heat to reflux for 20 hours, until the reaction solution is clear and does not separate into layers.

[0026] (2) Purification: evaporate the moisture in the reaction mixture under reduced pressure at 82° C. / 20 mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 4100 ml of absolute ethanol to obtain 508 grams of crude product. Then recrystallize with 8200ml of absolute ethanol, and obtain the pure product after filtration.

[0027] (3) Drying: the purified product was placed in a vacuum oven and dried for 3 hours at 80° C. / 100 mmHg to obtain 415 gram...

Embodiment 3

[0029] A preparation and purification method of ion-pair chromatography reagent sodium heptanesulfonate, comprising the following steps:

[0030] (1) Sulfonation: Add 630 g of anhydrous sodium sulfite and 2250 ml of water to a 10,000 ml three-necked flask equipped with a cooling reflux device and mechanical stirring, then add 627 g of bromoheptane and 8 g of tetrapropylammonium bromide, and heat to reflux for 24 hours, until the reaction solution is clear and does not separate into layers.

[0031] (2) Purification: evaporate the moisture in the reaction mixture under reduced pressure at 82° C. / 20 mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 7000 ml of absolute ethanol to obtain 870 grams of crude product. Then recrystallize with 14000ml of absolute ethanol, and obtain the pure product after filtration.

[0032] (3) Drying: the purified product was placed in a vacuum oven and dried for 4 hours at 80°C / 100mmHg to obtain 713 ...

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Abstract

The invention relates to a preparation method for an ion-pair chromatography reagent sodium heptanesulfonate. The preparation method comprises the following steps: sequentially adding anhydrous sodium sulfite, water, heptyl bromide and tetrapropylammonium bromide into a reaction vessel which is provided with a cooling reflux device and a mechanical stirrer; sulfonating for 16-24 hours; under a reducing pressure, evaporating moisture in a mixture obtained after finishing sulfonation reaction; smashing remained solid after being dried, and then adding into a Soxhlet extractor; extracting with absolute ethyl alcohol and obtaining a product, namely a rough product; re-crystallizing the rough product with the absolute ethyl alcohol; filtering for two times and then purifying, thereby obtaining a purified product; and lastly, drying the purified product for 2-4 hours, thereby obtaining an end product. According to the preparation method, during a sulfonation reaction process of sodium sulfite and heptyl bromide, the tetrapropylammonium bromide is taken as a catalyst, the activity of the heptyl bromide is enhanced, the sulfonation reaction is smoothly performed, the generation of by-products is reduced, the reaction time is obviously shortened, and the yield can reach 66%.

Description

technology field; [0001] The invention belongs to the field of chromatographic reagents, and relates to special reagents for high-performance liquid chromatography, in particular to a preparation method of sodium heptanesulfonate, an ion-pair chromatography reagent. Background technique; [0002] High performance liquid chromatography (HPLC) is widely used in bioengineering, food industry, pharmaceutical industry, petrochemical industry, environmental Supervision, commodity inspection, legal inspection and other disciplines. Ion-pair chromatography reagent Sodium heptanesulfonate is an indispensable special reagent for high-performance liquid chromatography. Its aqueous buffer system (mobile phase) composed of phosphate or acetate and organic modifier (methanol or acetonitrile) can be used in a certain A neutral association is formed in an equilibrium state, and an ion pair with an analyte of opposite charge is retained on the reversed-phase column to achieve the purpose of...

Claims

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Application Information

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