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天然单糖的存在对高糖样品中α-二羰基化合物定量的影响。使用不同衍生化反应的超高效液相色谱-单四极杆质谱法的比较研究。

Influence of the presence of natural monosaccharides in the quantification of α-dicarbonyl compounds in high content sugar samples. A comparative study by ultra-high performance liquid chromatography-single quadrupole mass spectrometry using different derivatization reactions.

作者信息

Hurtado-Sánchez María Del Carmen, Espinosa-Mansilla Anunciación, Durán-Merás Isabel

机构信息

Department of Analytical Chemistry and IACYS, University of Extremadura, Badajoz, 06006, Spain.

Department of Analytical Chemistry and IACYS, University of Extremadura, Badajoz, 06006, Spain.

出版信息

J Chromatogr A. 2015 Nov 27;1422:117-127. doi: 10.1016/j.chroma.2015.10.001. Epub 2015 Oct 9.

Abstract

The goal of this work is to evaluate the formation of side α-dicarbonyl compounds in high content sugar samples. These compounds may be originated from fructose and glucose, during different derivatization reactions. The formation of D-glucosone, 3-deoxyglucosone, glyoxal, and methylglyoxal, using three derivatization agents (5,6-diamino-2,4-hydroxypyrimidine, 2,4,5-triamine-6-hydroxypyrimidine, and o-phenylenediamine), and ultra-high pressure liquid chromatography in combination with MS detection, has been assessed in the presence of different levels of monosaccharides. 2,4,5-triamine-6-hydroxy-pyrimidine appears to be the most suitable for the analysis of α-dicarbonyl compounds, in this kind of food samples, and was selected as optimum reagent for the quantification of these compounds. The validation of the method was performed through the establishment of external standard calibration curves and analytical figures of merit, and it showed good linearity over a wide concentration range (r(2)>0.99), and limits of detection and quantification lower than 42μgL(-1) and 142μgL(-1), respectively. The validated method has been successfully applied to the determination of the target compounds in honey samples. The intraday and interday assay variability in the analysis of real samples was below 2.3 and 5.7%, respectively, for all analytes.

摘要

这项工作的目标是评估高糖样品中α-二羰基化合物的形成情况。这些化合物可能源于果糖和葡萄糖在不同衍生化反应过程中的产生。使用三种衍生化试剂(5,6-二氨基-2,4-二羟基嘧啶、2,4,5-三氨基-6-羟基嘧啶和邻苯二胺),并结合超高压液相色谱与质谱检测,在不同水平的单糖存在下,对D-葡萄糖酮、3-脱氧葡萄糖酮、乙二醛和甲基乙二醛的形成情况进行了评估。在这类食品样品中,2,4,5-三氨基-6-羟基嘧啶似乎最适合用于分析α-二羰基化合物,并被选为定量这些化合物的最佳试剂。通过建立外标校准曲线和分析性能指标对该方法进行了验证,结果表明该方法在较宽的浓度范围内具有良好的线性(r(2)>0.99),检测限和定量限分别低于42μgL(-1)和142μgL(-1)。该验证方法已成功应用于蜂蜜样品中目标化合物的测定。对于所有分析物,实际样品分析中的日内和日间测定变异分别低于2.3%和5.7%。

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