Development and Validation of a High-Performance Liquid Chromatography Method for the Determination of Diacetyl in Beer Using 4-Nitro-o-phenylenediamine as the Derivatization Reagent

Autor: Pingliang Li, Jiqiao Fan, Yongsong Cao, Shun He, Yuncong Zhu, Qiongbo Hu
Rok vydání: 2012
Předmět:
Zdroj: Journal of Agricultural and Food Chemistry. 60:3013-3019
ISSN: 1520-5118
0021-8561
DOI: 10.1021/jf3007163
Popis: Diacetyl is a natural byproduct of fermentation and known to be an important flavor compound in many food products. Because of the potential undesirable effects of diacetyl on health safety and beer flavor, determination of its concentration in beer samples is essential and its analytical methods have attracted close attention recently. The aim of the present work is to develop and validate a novel high-performance liquid chromatography method for the quantification of diacetyl in beer based on the derivatization reaction of diacetyl with 4-nitro-o-phenylenediamine (NPDA). After the derivatization with NPDA in pH 3.0 at 45 °C for 20 min, diacetyl was separated on a kromasil C(18) column at room temperature in the form of the resulting 6-nitro-2,3-dimethylquinoxaline and detected by the ultraviolet detector at 257 nm. The results showed that the correlation coefficient for the method was 0.9992 in the range of 0.0050-10.0 mg L(-1) and the limit of detection was 0.0008 mg L(-1) at a signal-to-noise ratio of 3. The applicability of the proposed method was evaluated in the analysis of beer samples with the recovery range of 94.0-99.0% and relative standard deviation range of 1.20-3.10%. The concentration levels of diacetyl detected in beer samples from 12 brands ranged from 0.034 to 0.110 mg L(-1). The proposed method showed efficient chromatographic separation, excellent linearity, and good repeatability that can be applied to quantification of diacetyl in beer samples.
Databáze: OpenAIRE