Abstract <p>The key requirements are outlined for an effective pre-column derivatization reagent used in the HPLC determination of chromophore-free organic compounds. Nitrofluorostyrenes, dichlorostyrenes, and diethyl 2-(4-nitrobenzylidene) malonate were studied as new reagents. Diethyl 2-(4-nitrobenzylidene) malonate was selected as the optimal reagent. 2-Methylmercaptoacetate was derivatized as a test analyte under mild conditions for 20 min at room temperature. The reaction proceeded to completion, forming a single product. The detection limit of 2-methylmercaptoacetate decreased by a factor of 67 (to 15 ng mL<sup>–1</sup>) compared to the initial value.</p>

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Synthesis of Diethyl 2-(4-Nitrobenzylidene) Malonate and Its Application as Derivatization Reagent in HPLC Detection of 2-Methylmercaptoacetate

  • D. A. Karpeev,
  • A. V. Pirogov

摘要

Abstract

The key requirements are outlined for an effective pre-column derivatization reagent used in the HPLC determination of chromophore-free organic compounds. Nitrofluorostyrenes, dichlorostyrenes, and diethyl 2-(4-nitrobenzylidene) malonate were studied as new reagents. Diethyl 2-(4-nitrobenzylidene) malonate was selected as the optimal reagent. 2-Methylmercaptoacetate was derivatized as a test analyte under mild conditions for 20 min at room temperature. The reaction proceeded to completion, forming a single product. The detection limit of 2-methylmercaptoacetate decreased by a factor of 67 (to 15 ng mL–1) compared to the initial value.