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Preparation method for liquid chromatography mass spectrometry (LC-MS)-grade high-purity acetonitrile reagents

A technology of liquid mass spectrometry and pure acetonitrile, which is applied in the direction of purification/separation of carboxylic acid nitriles, etc. It can solve the problems that the liquid mass spectrometry LC-MS grade high-purity acetonitrile reagent preparation method has not yet been found, so as to reduce dependence and process The equipment is easy to operate and stable in operation

Inactive Publication Date: 2012-10-24
天津康科德医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Through searching, no preparation method of LC-MS grade high-purity acetonitrile reagent for liquid mass spectrometry has been found

Method used

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  • Preparation method for liquid chromatography mass spectrometry (LC-MS)-grade high-purity acetonitrile reagents
  • Preparation method for liquid chromatography mass spectrometry (LC-MS)-grade high-purity acetonitrile reagents

Examples

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Embodiment 1

[0022] A liquid-mass chromatography LC-MS grade high-purity acetonitrile preparation method, the steps are as follows:

[0023] (1) Adsorption: At room temperature, the raw material acetonitrile with a content of about 99.5% is adsorbed sequentially through activated carbon, activated alumina and adsorption resin columns. The three adsorption columns are arranged in series. The particles of activated carbon, activated alumina and adsorption resin The diameters are 0.5~1.5mm, 0.1~0.5mm, and 0.2~1.0mm respectively; the adsorption flow rate is controlled to be about 100ml / min to remove impurities that absorb high-band ultraviolet rays.

[0024] (2) Oxidation: The effluent of the adsorption column flows into the oxidation kettle for oxidation. The oxidation kettle used in this embodiment is an energy-saving and environmentally friendly turbidization and volatilization reaction device. Add oxidant sodium persulfate or potassium iodate in the kettle, and the amount is 0.5~5% of the ...

Embodiment 2

[0029] A liquid-mass chromatography LC-MS grade high-purity acetonitrile preparation method, the steps are as follows:

[0030] (1) Adsorption: At room temperature, the raw material acetonitrile with a content of about 99.5% is adsorbed sequentially through activated carbon, activated alumina and adsorption resin columns. The three adsorption columns are arranged in series. The particles of activated carbon, activated alumina and adsorption resin The diameters are 0.5~1.5mm, 0.1~0.5mm and 0.2~1.0mm respectively; the adsorption flow rate is controlled at about 1000ml / min to remove impurities that absorb high-band UV.

[0031] (2) Oxidation: The effluent of the adsorption column flows into the oxidation kettle. The oxidation kettle used in this embodiment is an energy-saving and environment-friendly turbidization volatilization reaction device, and the oxidant potassium permanganate or ozone is added in the kettle, and its consumption is 100% of the effluent of the adsorption col...

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Abstract

The invention relates to a preparation method for liquid chromatography mass spectrometry (LC-MS)-grade high-purity acetonitrile reagents. The method includes steps: subjecting raw acetonitrile to adsorption by the aid of adsorbents such as activated carbon and activated alumina, oxidizing for purification, rectifying, dehydrating and drying by the aid of a molecular sieve, filtering by the aid of a microfiltration membrane, filling nitrogen for packaging, and obtaining the LC-MS-grade high-purity acetonitrile reagents. By the method, the recovery rate is more than 98%, the yield is more than 95%, the purity reaches to more than 99.99%, application requirements of clients on scientific researches and subject studies of the LC-MS-grade high-purity acetonitrile reagents can be met, domestic vacancies of production of the LC-MS-grade high-purity acetonitrile reagents can be filled, dependency on foreign reagents is lowered, high-quality reagents are provided for growing wide application of LC-MS quantitative analysis in high-tech fields such as biomedical research and development, clinic, food safety detection, pesticide residue analysis, veterinary drug residues, legal examiners, criminal investigations, doping detection, drug testing, agriculture and environment protection.

Description

technical field [0001] The invention belongs to the field of chemical reagents, and relates to acetonitrile reagents, in particular to a preparation method of LC-MS grade high-purity acetonitrile reagents for liquid mass spectrometry. Background technique [0002] The LC-MS grade high-purity acetonitrile reagent for liquid mass spectrometry has the characteristics of low ultraviolet absorption at ultra-low wavelength (200-220 nanometers), low noise background of chromatographic analysis, and high detection sensitivity. High-purity and high-quality reagents with detection limit. In recent years, the research and development of new chemical reagents has promoted new progress in methods, technologies and principles, and this advancement has played a related role in promoting many fields. With the advancement of science and technology and social development, the demand for reagents with low UV absorption, low suspended particles, low pH and low evaporation residue is increasing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34
Inventor 宋金链张玉芝
Owner 天津康科德医药化工有限公司
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