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Development of a Gas Chromatography-Mass Spectrometry Method for the Quantification of Glucaric Acid Derivatives in Beverage Substrates

机译:气相色谱-质谱法用于饮料基质中葡萄糖酸衍生物定量的开发

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摘要

A gas chromatography-mass spectrometry (GC-MS) method using the standard addition methodology was developed for the determination of glucuronolactone (GL) and glucuronic acid (DGuA) in four beverages categorized as detoxification, recovery, or energy drinks. The method features a precolumn derivatization step with a combination of BSTFA (N,O-bis(trimethylsilyl)trifluoroacetamide) and TMCS (trimethylchlorosilane) to silylate the analytes. The sample pretreatment required no extraction, filtration, or reduction step prior to the injection. The quantification of the analytes was performed using a five-point standard addition protocol. The proposed method presented excellent intraday precision (%RSD < 10) and linearity for GL calibration curves (correlation coefficients > 0.995) and acceptable linearity for DGuA calibration curves (correlation coefficients > 0.97). The estimated limits of detection (LOD) and quantification (LOQ) for GL ranged from 0.006 ppm to 0.14 ppm, and 0.02 ppm to 0.47 ppm, respectively. The estimated LOD and LOQ for DGuA determination ranged, respectively, from 0.06 ppm to 1.1 ppm and 0.2 ppm to 3.8 ppm. The results demonstrated that the method should be regarded as a reliable alternative to the simultaneous determination of GL and DGuA.
机译:开发了一种使用标准添加方法的气相色谱-质谱(GC-MS)方法,用于测定四种排毒,回收或能量饮料中的葡萄糖醛酸内酯(GL)和葡萄糖醛酸(DGuA)。该方法具有结合BSTFA(N,O-双(三甲基甲硅烷基)三氟乙酰胺)和TMCS(三甲基氯硅烷)的柱前衍生步骤,以使分析物甲硅烷基化。样品预处理在进样前无需提取,过滤或还原步骤。使用五点标准添加方案对分析物进行定量。所提出的方法具有出色的日内精度(%RSD <10)和GL校准曲线的线性(相关系数> 0.995),以及DGuA校准曲线的可接受的线性(相关系数> 0.97)。 GL的估计检出限(LOD)和定量限(LOQ)分别为0.006 ppm至0.14 0.1ppm和0.02,ppm至0.47 ppm。用于DGuA测定的估计LOD和LOQ分别为0.06 ppm至1.1 µppm和0.2 µppm至3.8 µppm。结果表明,该方法应被视为同时测定GL和DGuA的可靠替代方法。

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