Preparation method of ion pair chromatographic-grade reagent sodium 1-heptanesulfonate

A technology of sodium heptanesulfonate and ion-pair chromatography, which is applied in the field of preparation technology of ion-pair chromatography grade reagent 1-sodium heptanesulfonate, can solve the problems of high cost, inability to meet the requirements of scientific research experiments, complicated process, etc. Achieve the effect of simple operation, novel process and low ultraviolet absorption

Inactive Publication Date: 2014-02-05
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of commercially available sodium 1-heptane sulfonate reaches 98%, and there are still trace impurities with high ultraviolet absorption, which cannot meet the requirements of relevant scientific research experiments
[0003] The development of domestic ion-pair chromatographic grade reagents lags behind the needs of current scientific research and development, although patent CN101693677, CN102432507 provides a raw material with 1-bromoheptane, the method for preparing ion-pair chromatographic grade 1-heptanesulfonate sodium by synthetic means , but involves multiple processes such as chemical reaction, product post-treatment, crude product purification, etc., the process is complicated and the cost is high

Method used

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  • Preparation method of ion pair chromatographic-grade reagent sodium 1-heptanesulfonate
  • Preparation method of ion pair chromatographic-grade reagent sodium 1-heptanesulfonate

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Embodiment 1

[0017] A kind of preparation process method of ion-pair chromatographic grade reagent 1-sodium heptanesulfonate, the steps are as follows:

[0018] (1) Put 40 g of sodium 1-heptanesulfonate with a purity of 98% into 160 ml of acetone, and perform ultrasonic irradiation and vibration. The ultrasonic frequency is set to 35 KHz, the temperature is controlled at 20°C to 30°C, and the ultrasonic time is 2h.

[0019] (2) Cool the mixture obtained in step (1) to room temperature naturally, carry out suction filtration under reduced pressure, and press dry the filter cake. The mother liquor was distilled under reduced pressure to recover the organic solvent.

[0020] (3) Put the obtained filter cake solid into 160ml of ethanol-water mixture, the mass ratio of ethanol and water is 50:1, heat and reflux and stir for 2h, filter while it is hot, cool the filtrate naturally, and freeze at 0°C to precipitate crystals.

[0021] (4) The crystals obtained in step (3) were filtered under reduc...

Embodiment 2

[0025] A kind of preparation process method of ion-pair chromatographic grade reagent 1-sodium heptanesulfonate, the steps are as follows:

[0026] (1) 100 g of raw material 1-heptane sulfonate with a purity of 98% was put into 800 ml of acetone, and subjected to ultrasonic irradiation and oscillation. The ultrasonic frequency was set at 53 KHz, the temperature was controlled at 40°C to 50°C, and the ultrasonic time was 8 hours.

[0027] (2) Cool the mixture in step (1) to room temperature naturally, perform suction filtration under reduced pressure, and press dry the filter cake. The mother liquor was distilled under reduced pressure to recover the organic solvent.

[0028] (3) Put the obtained filter cake solid into 800ml ethanol-water mixture, the mass ratio of ethanol and water is 100:1, heat and reflux and stir for 5h, filter while it is hot, cool the filtrate naturally, and freeze at 10°C to precipitate crystals.

[0029] (4) The crystals obtained in step (3) were filte...

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Abstract

The invention provides a preparation method of an ion pair chromatographic-grade reagent sodium 1-heptanesulfonate. The preparation method is characterized in that specific steps are as follows: adding material sodium 1-heptanesulfonate into acetone, carrying out ultrasonic-wave irradiation oscillation, cooling to the room temperature, and reducing pressure for suction filtration; adding obtained filter cake solid into alcohol-water mixed liquor, heating, refluxing and stirring, filtering when the liquor is hot, naturally cooling filtrate, and freezing at low temperature to separate out crystals; reducing the pressure for suction filtration, collecting the crystals, and drying to obtain ion pair chromatographic-grade reagent sodium 1-heptanesulfonate. The preparation method disclosed by the invention sufficiently utilizes advantages of ultrasonic-wave cavitation effect, and is combined with a freezing crystallization method to achieve the purpose of purifying sodium 1-heptanesulfonate.

Description

technical field [0001] The invention relates to a special reagent for high-performance liquid chromatography, in particular to a preparation process of ion-pair chromatography grade reagent 1-sodium heptanesulfonate. Background technique [0002] Ion chromatography (Ion Chromatograhpy) is a kind of high performance liquid chromatography (HPLC). Because of its fast analysis speed, high detection sensitivity, good selectivity and high stability, it is widely used in food, medicine, petrochemical, environmental geology and other fields. Ion-pair chromatography reagent 1-sodium heptanesulfonate is an essential special reagent for high performance liquid chromatography. Commercially available sodium 1-heptane sulfonate has a content of 98%, but there are still trace impurities with high ultraviolet absorption, which cannot meet the requirements of relevant scientific research experiments. [0003] The development of domestic ion-pair chromatography grade reagents lags behind th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/04C07C303/44
Inventor 凌青
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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