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Development and Application of a New QuEChERS Method in UHPLC-QqQ-MS/MS to Detect Seven Biogenic Amines in Chinese Wines

机译:UHPLC-QqQ-MS / MS中QuEChERS新方法的开发和应用可检测中国葡萄酒中的7种生物胺

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摘要

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.
机译:这项研究的目的是开发和验证一种同时测定七种类型(尸胺,CAD,己胺,HEX,组胺,HIS,苯乙胺,PEA,腐胺,PUT,酪胺,TYR)的改进,简单且灵敏的方法。葡萄酒基质中生物胺的含量。因此,研究了改良的QuEChERS与超高效液相色谱结合三重四极杆质谱(UHPLC-QqQ-MS / MS)方法。进行了UHPLC-QqQ-MS / MS分离和QuEChERS程序的优化。在最佳条件下,整个分离过程的出色色谱性能在6.3分钟的分析时间内即可实现。同时,回收率在77.2%至101.7%之间,而相对标准偏差(RSD)则保持在0.0%至9.4%之间。检出限(LOD,0.50–1.00 µg / L)和定量限(LOQ,1.65–3.30 µg / L)均低于食品基质法规所允许的水平,这表明该高效方法具有很高的灵敏度和适用性方法。这项经过验证的方法还用于初步研究中,以分析来自河西走廊地区(中国西北地区)的81个葡萄酒样品中的BA,并在样品中不同程度地检测了CAD,HEX,HIS,PEA,PUT和TYR。但是,与现有标准相比,所有81个葡萄酒样品中的BA均未超过规定的限值或有毒剂量(2–40 mg / L)。此外,还使用Pearson相关分析进行统计,并根据葡萄酒参数(储存时间,葡萄品种,葡萄酒类型和基本理化指标)评估其浓度。结果表明,在7种BAs中,HIS的浓度与酒度和葡萄品种有一定的相关性。另外,PEA的含量与葡萄酒的pH值和葡萄酒的储存时间有一定的相关性。值得注意的是,这似乎是有关QuEChERS-UHPLC-QqQ-MS / MS在该地区葡萄酒中BA的分析中的首次报道。

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