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<p>During the registration procedure of a drug substance, the actual and potential impurities must be summarized in a legal documentation. Diketene is a reactive chemical compound which is used for the introduction of an acetoacetyl structural unit into organic compounds. Since this material commonly used as a reagent in the pharmaceutical industry, it is a potential impurity of certain drug substances. The aim of this work was to develop and validate a suitable method for the analysis of diketene by means of decomposition headspace gas chromatography. The product of the derivatization reaction is acetone, which can be easily measured by gas chromatography. Various parameters have been integrated into the elaborated limit test validation, such as specificity, detection limit (LD), quantification limit (LQ), system precision, recovery at limit level, robustness and solution stability. The limits of detection and quantification are 60 and 200&#xa0;ppm, respectively. Using the above-mentioned new analytical method, the concentration of diketene can be determined accurately. These precise measurements are necessary for the appropriate characterization of the drug substance, which is a prerequisite step of a marketing authorization for the finished product.</p>

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Measurement of Diketene Using In Situ Derivatization-Headspace-Gas Chromatography

  • 期刊论文

  • 发表日期：

    2025年3月5日

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  • Noémi Göröcs,
  • Balázs Volk

摘要

During the registration procedure of a drug substance, the actual and potential impurities must be summarized in a legal documentation. Diketene is a reactive chemical compound which is used for the introduction of an acetoacetyl structural unit into organic compounds. Since this material commonly used as a reagent in the pharmaceutical industry, it is a potential impurity of certain drug substances. The aim of this work was to develop and validate a suitable method for the analysis of diketene by means of decomposition headspace gas chromatography. The product of the derivatization reaction is acetone, which can be easily measured by gas chromatography. Various parameters have been integrated into the elaborated limit test validation, such as specificity, detection limit (LD), quantification limit (LQ), system precision, recovery at limit level, robustness and solution stability. The limits of detection and quantification are 60 and 200 ppm, respectively. Using the above-mentioned new analytical method, the concentration of diketene can be determined accurately. These precise measurements are necessary for the appropriate characterization of the drug substance, which is a prerequisite step of a marketing authorization for the finished product.