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  • Method development by GC-ECD and HS-SPME-GC-MS for beer volatile analysis.

Method development by GC-ECD and HS-SPME-GC-MS for beer volatile analysis.

Food chemistry (2014-08-26)
Gisele C da Silva, Abner A S da Silva, Larissa S N da Silva, Ronoel Luiz de O Godoy, Luciana C Nogueira, Simone L Quitério, Renata S L Raices
ABSTRACT

Two methods for the extraction, identification and quantification of the highest occurrence and lowest perception threshold off-flavours in fifteen different samples of Brazilian Pilsner beers were developed. For this purpose, headspace solid phase microextraction in combination with a gas chromatography coupled to a mass spectrometric detection (HS-SPME-GC-MS) as well as headspace extraction in combination with a gas chromatography coupled to electron capture detection (HS-GC-ECD) were evaluated. The first and the second methods were used for esters and vicinal diketones analysis, respectively. All data were comprehended below the taster's threshold detection limit: ethyl acetate 39.48 ng mL(-1) (RSD mean value 4.2%), isoamyl acetate 3.88 ng mL(-1) (RSD mean value 3.4%), ethyl hexanoate 0.61 ng mL(-1) (RSD mean value 3.1%) and 2,3-butanedione 0.10 ng mL(-1) (RSD mean value 2.9%). The validated method demonstrated to be useful for the analysis of highest incidence beer off-flavours.

MATERIALS
Product Number
Brand
Product Description

Supelco
Isopentyl acetate, analytical standard
Sigma-Aldrich
Isopentyl acetate, anhydrous, ≥99%
Sigma-Aldrich
Ethyl hexanoate, ≥98%, FCC, FG
Supelco
2,3-Butanedione, analytical standard
Sigma-Aldrich
2,3-Pentanedione, ≥96%, FCC, FG
Sigma-Aldrich
Poly(dimethylsiloxane), viscosity 1.0 cSt (25 °C)
Sigma-Aldrich
Hexamethyldisiloxane, viscosity 0.65 cSt (25 °C)
Sigma-Aldrich
Ethyl hexanoate, ≥99%
Sigma-Aldrich
2,3-Butanedione, 97%
Supelco
Ethyl hexanoate, analytical standard
Sigma-Aldrich
2,3-Pentanedione, natural, ≥96%, FG
Supelco
2,3-Pentanedione, analytical standard
Sigma-Aldrich
2,3-Pentanedione, 97%
Sigma-Aldrich
Ethyl hexanoate, natural, ≥98%, FCC, FG
Sigma-Aldrich
Isopentyl acetate, mixture of isomers, reagent grade, 98%
Supelco
Ethyl acetate, analytical standard
Sigma-Aldrich
Ethyl acetate, ReagentPlus®, ≥99.8%
Sigma-Aldrich
Ethyl acetate, anhydrous, 99.8%
Sigma-Aldrich
Isoamyl acetate, natural, ≥97%, FCC, FG
Sigma-Aldrich
Isoamyl acetate, ≥95%, FCC, FG
Sigma-Aldrich
Ethyl acetate, ≥99%, FCC, FG
Sigma-Aldrich
Ethyl acetate, natural, ≥99%, FCC, FG
Sigma-Aldrich
Ethyl acetate
Sigma-Aldrich
Ethyl acetate
Sigma-Aldrich
Ethyl acetate, biotech. grade, ≥99.8%
Sigma-Aldrich
Ethyl acetate, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
Sigma-Aldrich
Ethyl acetate, suitable for HPLC, ≥99.8%
Supelco
Ethyl Acetate, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ethyl acetate, ACS reagent, ≥99.5%
Sigma-Aldrich
Ethyl acetate, ACS reagent, ≥99.5%