Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.
A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO2on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R2> 0.98) within the tested range (1-50 ng l-1). Recoveries were evaluated at three different levels (1, 5 and 50 ng l-1) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l-1, which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l-1.
a Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence, ceiA3 , Almería , Spain.
Ana
A
Ruiz-Delgado
a Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence, ceiA3 , Almería , Spain.
Francisco Javier
FJ
Arrebola-Liébanas
a Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence, ceiA3 , Almería , Spain.
Roberto
R
Romero-González
a Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence, ceiA3 , Almería , Spain.
Rosalía
R
López-Ruiz
a Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence, ceiA3 , Almería , Spain.
Antonia
A
Garrido Frenich
D000434:Alcoholic Beverages / Q000032:analysis*; D000840:Anisoles / Q000032:analysis*; D002849:Chromatography, Gas; D052617:Solid Phase Microextraction; D053719:Tandem Mass Spectrometry
D000840:Anisoles
GC-MS/MS; HS-SPME; Haloanisoles; cork taint