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反相高效液相色谱数据多变量分析发酵食品中的有机酸。

Multivariate analysis of organic acids in fermented food from reversed-phase high-performance liquid chromatography data.

机构信息

Laboratorio de Biotecnología e Inocuidad de los Alimentos. Municipalidad de Granadero Baigorria - Facultad de Ciencias Bioquímicas y Farmacéuticas (UNR, Universidad Nacional de Rosario), Suipacha 531, S2000LRK Rosario, Argentina; Instituto de Química de Rosario (IQUIR, UNR-CONICET), Suipacha 570, S2000LRK Rosario, Argentina.

Laboratorio de Biotecnología e Inocuidad de los Alimentos. Municipalidad de Granadero Baigorria - Facultad de Ciencias Bioquímicas y Farmacéuticas (UNR, Universidad Nacional de Rosario), Suipacha 531, S2000LRK Rosario, Argentina; Instituto de Biología de Rosario (IBR, UNR-CONICET), Suipacha 590, S2000LRK Rosario, Argentina.

出版信息

Talanta. 2018 Feb 1;178:15-23. doi: 10.1016/j.talanta.2017.09.005. Epub 2017 Sep 5.

Abstract

Multivariate calibration coupled to RP-HPLC with diode array detection (HPLC-DAD) was applied to the identification and the quantitative evaluation of the short chain organic acids (malic, oxalic, formic, lactic, acetic, citric, pyruvic, succinic, tartaric, propionic and α-cetoglutaric) in fermented food. The goal of the present study was to get the successful resolution of a system in the combined occurrence of strongly coeluting peaks, of distortions in the time sensors among chromatograms, and of the presence of unexpected compounds not included in the calibration step. Second-order HPLC-DAD data matrices were obtained in a short time (10min) on a C18 column with a chromatographic system operating in isocratic mode (mobile phase was 20mmolL phosphate buffer at pH 2.20) and a flow-rate of 1.0mLmin at room temperature. Parallel factor analysis (PARAFAC) and unfolded partial least-squares combined with residual bilinearization (U-PLS/RBL) were the second-order calibration algorithms select for data processing. The performance of the analytical parameters was good with an outstanding limit of detection (LODs) for acids ranging from 0.15 to 10.0mmolL in the validation samples. The improved method was applied to the analysis of many dairy products (yoghurt, cultured milk and cheese) and wine. The method was shown as an effective means for determining and following acid contents in fermented food and was characterized by reducibility with simple, high resolution and rapid procedure without derivatization of analytes.

摘要

多元校正结合反相高效液相色谱法与二极管阵列检测(HPLC-DAD)被应用于发酵食品中短链有机酸(苹果酸、草酸、甲酸、乳酸、乙酸、柠檬酸、丙酮酸、琥珀酸、酒石酸、丙酸和α-酮戊二酸)的鉴定和定量评价。本研究的目的是成功解决一个系统中强烈共洗脱峰、色谱图中时间传感器失真以及校准步骤中未包含的意外化合物存在的问题。在室温下,使用 C18 柱和等度模式的色谱系统(流动相为 20mmol/L 磷酸盐缓冲液,pH 值为 2.20),在 10min 内获得了二阶 HPLC-DAD 数据矩阵,流速为 1.0mL/min。平行因子分析(PARAFAC)和未展开偏最小二乘法结合残余双线性化(U-PLS/RBL)是用于数据处理的二阶校正算法。分析参数的性能良好,在验证样品中,酸的检出限(LOD)低至 0.15-10.0mmol/L。改进后的方法应用于许多乳制品(酸奶、发酵乳和奶酪)和葡萄酒的分析。该方法是一种有效确定和跟踪发酵食品中酸含量的方法,具有简单、高分辨率和快速的特点,无需对分析物进行衍生化。

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