alexa Determination of polar alkylating agents as thiocyanate isothiocyanate derivatives by reaction headspace gas chromatography
Chemical Engineering

Chemical Engineering

Journal of Chromatography & Separation Techniques

Author(s): Christopher R Lee, Florence Guivarch, Cline Nguyen Van Dau, Dominique Tessier, Ante M Krstulovic

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We report a new method for the determination of the methyl, ethyl and isopropyl esters of methanesulfonic acid, and of dimethyl sulfate. Derivatisation with aqueous sodium thiocyanate gives a mixture of the corresponding alkylthiocyanates and alkylisothiocyanates which, unlike the underivatised analytes, are readily analysed by GC. On-column isomerisation is negligible. These lower alkyl derivatives are sufficiently volatile for static reaction headspace analysis, and detection limits obtained by electron impact MS are below 0.05 µg ml−1 with respect to the injection solution. The method was used to demonstrate that levels of methanesulfonic acid esters in a drug substance (a mesylate salt that had been processed using methanol and ethanol) are below 1 µg g−1.

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This article was published in Analyst and referenced in Journal of Chromatography & Separation Techniques

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