GC/FID determination method for contents of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid

A technology of alkyl methanesulfonate and methyl methanesulfonate, applied in the field of medicine and chemical industry, can solve problems such as human health threat and DNA mutation, and achieve the effect of low cost and scientific determination method

Pending Publication Date: 2021-03-16
JIANGSU ALPHA PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Clinical studies have found that alkyl mesylate can directly undergo alkylation reactions with biomacromolecules (DNAs, RNAs, and proteins), which may cause DNA mutations
Methyl mesylat

Method used

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  • GC/FID determination method for contents of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid
  • GC/FID determination method for contents of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid
  • GC/FID determination method for contents of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid

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Embodiment Construction

[0029] The present invention is further described by the following specific examples, but does not limit the present invention.

[0030] 1. Instruments, reagents and instrument working conditions

[0031] 1) Instrument

[0032] Gas chromatograph (Agilent7890A), equipped with hydrogen flame ion detector; BSA224S electronic balance (sensitivity: 0.01mg, Sartorius Scientific Instrument Co., Ltd.): Hy-8A speed-adjustable oscillator (Changzhou Guohua Electric Co., Ltd.), Xiangli Cenless 16R desktop high-speed refrigerated centrifuge.

[0033] 2) Reagents

[0034] Dichloromethane (chromatographically pure), isopropyl ethanesulfonate (internal standard, CAS: 14245-62-6, purity ≥ 99%), methyl methanesulfonate, (CAS: 66-27-3, purity ≥ 99%) %), ethyl methanesulfonate (CAS: 62-50-0, purity ≥ 99%), isopropyl methanesulfonate (CAS: 926-06-7, purity ≥ 99%), methanesulfonyl chloride (CAS: 558-25-8 purity ≥ 99%), anhydrous magnesium sulfate (analytical grade).

[0035] 3) The gas chromat...

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Abstract

The invention discloses a GC/FID (Gas Chromatography/Flame Ionization Detector) determination method for contents of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid (MsOH),namely methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS), isopropyl methanesulfonate (IMS) and methanesulfonyl chloride (MsCl); and the method is characterized in that the methanesulfonic acid is subjected to water and dichloromethane extraction and layering treatment; gas chromatography and a hydrogen flame ion detector (GC/FID) are adopted, and the contents of methyl methanesulfonate,ethyl methanesulfonate, isopropyl methanesulfonate and methylsulfonyl chloride in methanesulfonic acid are detected quantitatively by adopting an internal standard method. According to the detectionmethod provided by the invention, the methyl methanesulfonate MMS, the ethyl methanesulfonate EMS, the isopropyl methanesulfonate IMS and the methylsulfonyl chloride MsCl are combined and detected inone method, so that the detection efficiency is improved, and the extraction method is simple, effective, high in sensitivity and good in recovery rate.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a GC / FID method for determining the content of alkyl methanesulfonate and methanesulfonyl chloride in methanesulfonic acid. Background technique [0002] Alkyl methanesulfonate, such as methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS), isopropyl methanesulfonate (IMS), is methanesulfonic acid mixed with methanol, ethanol, isopropanol or other Esters formed from lower alcohols. In particular, lower alcohols are used in the presence of methanesulfonic acid (MsOH) or methanesulfonyl chloride (MsCL) in active pharmaceutical ingredients formed as mesylate or mesylate esters or during their synthesis, Alkyl methanesulfonate would be considered a potential impurity. Clinical studies have found that alkyl methanesulfonate can directly undergo alkylation reactions with biomacromolecules (DNAs, RNAs and proteins), which may cause DNA mutations. Methyl methanesulf...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/68
CPCG01N30/02G01N30/06G01N30/68G01N2030/025G01N2030/045G01N2030/062
Inventor 石利平陈本顺叶金星李大伟徐春涛马骧刘晶钱若灿汝彬彬张闯占继田陆梦云
Owner JIANGSU ALPHA PHARM CO LTD
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