Direct accurate analysis of cysteinylated and glutathionylated precursors of 4-mercapto-4-methyl-2-pentanone and 3-mercaptohexan-1-ol in must by ultrahigh performance liquid chromatography coupled to mass spectrometry

  1. Concejero, B. 1
  2. Peña-Gallego, A. 1
  3. Fernandez-Zurbano, P. 2
  4. Hernández-Orte, P. 1
  5. Ferreira, V. 1
  1. 1 Universidad de Zaragoza
    info

    Universidad de Zaragoza

    Zaragoza, España

    ROR https://ror.org/012a91z28

  2. 2 Instituto de Ciencias de la Vid y del Vino
    info

    Instituto de Ciencias de la Vid y del Vino

    Logroño, España

    ROR https://ror.org/01rm2sw78

Revista:
Analytica Chimica Acta

ISSN: 0003-2670

Ano de publicación: 2014

Volume: 812

Páxinas: 250-257

Tipo: Artigo

DOI: 10.1016/J.ACA.2014.01.004 SCOPUS: 2-s2.0-84894904350 GOOGLE SCHOLAR

Outras publicacións en: Analytica Chimica Acta

Resumo

A direct method for the quantitative determination in grapes of four known precursors of the varietal aromas of the thiol character of wine has been optimized and validated. A small volume of centrifuged and filtered must is directly injected in the ultrahigh liquid performance chromatography coupled to mass spectrometry system (UHPLC-MS-MS). Must sugars and other early eluting polar compounds are diverted to the waste, not entering the ion source. Cysteinyl (CYS) and glutathionyl (GLU) precursors from 3-mercaptohexanol (3MH) and 4-mercapto-4-methylpentanone (4M4MP) are separated in 5 min rendering narrow peaks (W1/2 < 9 s). No system performance degradation has been noticed in series of more than 200 injections. A standard addition procedure using the consecutive injection of a spiked sample made it possible to satisfactorily correct for matrix effects, with recoveries very close to 100% in all cases. Intermediate reproducibility was satisfactory (RSD between 1 and 10%), except for the glutathione-4-mercapto-4-methyl-2-pentanone (GLUMP) precursor, for which this value is around 20%. The limits of detection in real-must were below 1 μg L-1 for the precursors of the 4M4MP and for cysteine-3-mercaptohexan-1-ol (CYSMH) and glutathione-3-mercaptohexan-1-ol (GLUMH), 2 and 7 μg L-1, respectively, what is enough for the determination of these precursors in musts of any variety. © 2014 Elsevier B.V. All rights reserved.