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9 Fluorenylmethyl Chloroformate

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Pilar Campíns-falcó – One of the best experts on this subject based on the ideXlab platform.

Rosa Herráez-hernández – One of the best experts on this subject based on the ideXlab platform.

  • An evaluation of solid phase microextraction for aliphatic amines using derivatization with 9Fluorenylmethyl Chloroformate and liquid chromatography.
    Journal of chromatography. A, 2006
    Co-Authors: Rosa Herráez-hernández, C Cháfer-pericás, J Verdú-andrés, Pilar Campíns-falcó

    The reliability of SPME combined with a chemical reaction for the analysis of short-chain aliphatic amines by liquid chromatography has been investigated. Different options to couple SPME and derivatization have been tested and compared: (i) derivatization of the analytes in solution followed by the extraction of the derivatives, (ii) extraction of the analytes and subsequent derivatization by immersing the SPME fibre onto a solution of the reagent, and (iii) extraction/derivatization of the analytes using fibres previously coated with the reagent. Methylamine (MA), dimethylamine (DMA) and trimethylamine (TMA) have been selected as a model of primary, secondary and tertiary amines, respectively. The analytes have been derivatized with the fluorogenic reagent 9Fluorenylmethyl Chloroformate (FMOC), and the fibre coating was Carbowax-templated resin (CW-TR). The employment of fibres coated with FMOC to extract and derivatize the analytes was the best option, as compared with the other approaches tested the sensitivity was considerably improved. On the basis of these studies, a new procedure for the determination of MA, DMA and TMA in water is presented. To demonstrate the utility of the proposed conditions data on linearity, accuracy, repeatability and sensitivity are given. Results of the determination of the amines in tap, river and waste water are also presented.

  • A new selective method for dimethylamine in water analysis by liquid chromatography using solid-phase microextraction and two-stage derivatization with o-phthalaldialdehyde and 9Fluorenylmethyl Chloroformate.
    Talanta, 2005
    Co-Authors: Consuelo Cháfer-pericás, Rosa Herráez-hernández, Pilar Campíns-falcó

    Abstract A new method is presented for the determination of DMA in water as its 9Fluorenylmethyl Chloroformate (FMOC) derivative using solid-phase microextraction (SPME) and liquid chromatography. The method is based on the employment of SPME fibres coated with carbowax-templated resin (CW-TR) for analyte extraction and derivatization. The fibres were successively immersed in the samples, in a solution of o -phthalaldialdehyde and N -acethyl- l -cysteine (OPA–NAC) and finally, in a solution of FMOC. OPA–NAC reacted on the fibre with possible primary aliphatic amines present in the samples, particularly with PA which is a direct interferent in the determination of DMA with FMOC. In such a way, the formation of PA–FMOC during the second stage was prevented, and thus the method was selective for DMA. The proposed procedure was applied to the determination of DMA in the 1.0–10.0 μg/mL range. The method provided suitable linearity, accuracy and reproducibility, and limits of detection and quantification of 0.3 and 1.0 μg/mL, respectively. The applicability of the method for the determination of DMA in different types of water is shown.

  • Analysis of methylamine by solid-phase microextraction and HPLC after on-fibre derivatization with 9Fluorenylmethyl Chloroformate
    Analytica Chimica Acta, 2004
    Co-Authors: Rosa Herráez-hernández, Consuelo Cháfer-pericás, Pilar Campíns-falcó

    Abstract A method for the determination of methylamine (MA) in aqueous matrices is reported which uses solid-phase microextraction (SPME) for enrichment and derivatization of the analyte, and high performance liquid chromatography (HPLC). The fluorogenic reagent 9Fluorenylmethyl Chloroformate (FMOC) has been used for derivatization. The SPME fibres were successively immersed in the samples and in the derivatization solutions to extract MA and FMOC, respectively. After a defined time of reaction, the derivatized analyte was desorbed into the chromatographic system, and chromatographed in a LiChrosphere 100 RP18, 125 mm ×4 mm i.d., 5 μm, column under gradient elution. In order to improve the MA-FMOC peak profile, a precolumn ( 20 mm ×2.1 mm i.d., packed with Hypersil C18 phase, 30 μm) was connected on-line to the analytical column by means of a switching valve. The experimental conditions (including fibre coating, times of adsorption, reaction and desorption, and concentration of reagent) have been optimised, and the results have been compared with those achieved by using a method previously validated for aliphatic amines in which extraction and derivatization were carried into C18 solid-phase extraction (SPE) cartridges. Although less sensitive, the SPME based method allowed the quantification of MA over the range 2.5–10.0 μg/ml with linearity, reproducibility and accuracy comparable to that of the SPE based method, the limit of detection being 0.75 μg/ml. The main advantages of the proposed SPME procedure are: sample handling involved in the extraction and derivatization steps was considerably reduced, it was free organic solvent and non-destructive. Moreover, the proposed conditions allowed the selective determination of MA in the presence of other primary and secondary short-chain aliphatic amines. The utility of the proposed procedure for the quantification of MA in different types of waters is discussed.

Gholamreza Bahrami – One of the best experts on this subject based on the ideXlab platform.

Xianliang Zhou – One of the best experts on this subject based on the ideXlab platform.

Ying Zhang – One of the best experts on this subject based on the ideXlab platform.