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Determination of 2-alkylcyclobutanones by combining precolumn derivatization with 1-naphthalenyl hydrazine and ultra-performance liquid chromatography with fluorescence detection

机译:结合柱前衍生化与1-萘肼和超高效液相色谱-荧光检测法测定2-烷基环丁酮

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摘要

2-Alkylcyclobutanones (2-ACBs) are uniquely formed when triglycerides-containing food products are exposed to ionizing radiation. Thus, 2-ACBs have been used as marker molecules to identify irradiated food. Most methods to determine 2-ACBs involve mass spectrometric detection after chromatographic separation. The spectrofluorometer is rarely used to determine 2-ACBs because these molecules do not fluoresce. In this study, we developed an ultra-performance liquid chromatography (UPLC) method to determine 2-ACBs. 2-ACBs were converted into fluorophores after reacting with 1-naphthalenyl hydrazine to facilitate their sensitive and selective detection using a fluorescence detector (FLD). Analysis of 2-ACBs using our developed UPLC-FLD method allows sensitive determination of 2-ACBs at a detection limit of 2 ng 2-ACBs per g of fat (30 pg/injection), which is significantly lower than that of existing analytical methods. After validation for trueness and precision, the method was applied to gamma-irradiated chicken samples to determine their 2-ACB content. Comparative studies employing liquid chromatography-tandem mass spectrometric method revealed no systematic difference between the two methods, thereby demonstrating that the proposed UPLC-FLD method can be suitably used to determine 2-ACBs in irradiated foodstuffs.
机译:当含甘油三酸酯的食品暴露于电离辐射时,会独特地形成2-烷基环丁酮(2-ACB)。因此,2-ACB已被用作标记分子以识别受辐照的食物。确定2-ACB的大多数方法都涉及色谱分离后的质谱检测。光谱荧光计很少用于测定2-ACB,因为这些分子不发荧光。在这项研究中,我们开发了一种超高效液相色谱(UPLC)方法来测定2-ACB。在与1-萘肼反应后,将2-ACBs转换为荧光团,以利于使用荧光检测器(FLD)进行灵敏和选择性的检测。使用我们开发的UPLC-FLD方法分析2-ACB可以灵敏地测定2-ACB,检测限为每克脂肪2 ng 2-ACB(每次进样30 pg),这大大低于现有的分析方法。经过真实性和精确性验证后,将该方法应用于经伽马射线辐照的鸡肉样品,以确定其2-ACB含量。使用液相色谱-串联质谱法进行的比较研究表明,这两种方法之间没有系统上的区别,从而证明了所提出的UPLC-FLD方法可适用于测定辐照食品中的2-ACB。

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