Abstract
The aim of this study was to develop and validate an improved, simple, and sensitive method for the simultaneous determination of seven types (cadaverine, CAD; hexylamine, HEX; histamine, HIS; phenylethylamine, PEA; putrescine, PUT; tyramine, TYR) of biogenic amines (BAs) in wine matrices. For this reason, a modified QuEChERS combined with ultra-performance liquid chromatography coupled to a triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS) method was investigated. The optimization of UHPLC-QqQ-MS/MS separation and QuEChERS procedure was performed. Under optimum conditions, the excellent chromatographic performance of the whole separation was accomplished within 6.3 min analyzing time. Meanwhile, the recoveries ranged from 77.2% to 101.7%, while relative standard deviation (RSD) remained between 0.0% and 9.4%. The limit of detection (LOD, 0.50–1.00 µg/L) and the limit of quantification (LOQ, 1.65–3.30 µg/L) were lower than those permitted by legislation in food matrices, which demonstrated the high sensitivity and applicability of this efficient method. This validated method was also applied in a pilot study to analyze BAs in 81 wine samples from Hexi Corridor Region (Gansu Province, Northwest China), CAD, HEX, HIS, PEA, PUT, and TYR were detected to varying degrees in the samples. However, when compared with the existing standards, the BAs in all 81 wine samples did not exceed the prescribed limit value or toxic dose (2–40 mg/L). Moreover, a statistical approach was also conducted using Pearson correlation analysis, and to evaluate their concentrations in terms of wine parameters (storage time, grape variety, wine type, and basic physicochemical index). The results showed that, among the seven kinds of BAs, the concentration of HIS had a certain correlation with alcoholic degree and grape variety. In addition, the level of PEA had a certain correlation with the wine pH and wine storage time. It is worth noting that this seems to be the first report regarding the application of QuEChERS-UHPLC-QqQ-MS/MS in the analysis of BAs in wine in this region.
Highlights
Biogenic amines (BAs) are toxic nitrogenous organic compounds that are mainly produced by microbial decarboxylation of free amino acids
The results showed that, among the seven kinds of biogenic amines (BAs), the concentration of HIS had a certain correlation with alcoholic degree (p < 0.01) and grape variety (p < 0.05)
The optimization of MS/MS parameter, UHPLC separation, and QuEChERS procedure, which includes matrix pH condition, solvent, salt type and amount, clean-up agent, were performed, and the whole separation of BAs was accomplished within 6.3 min of analyzing time
Summary
Biogenic amines (BAs) are toxic nitrogenous organic compounds that are mainly produced by microbial decarboxylation of free amino acids. Previous research found that the BAs appeared in a wide variety of food, such as meat [1] and fishery products [2]. There is general agreement that yeasts make a less significant contribution than lactic acid bacteria to the final concentration of BAs in wine [3]. By their structure, BAs can be divided into three well-defined categories, which are aliphatic, aromatic, and heterocyclic amines [4].
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