Analytical Chemistry, Nutrition and Food Science Department, University of Salamanca, Plaza de los Caídos s/n, 37008 Salamanca, Spain.
Analytical Chemistry, Nutrition and Food Science Department, University of Salamanca, Plaza de los Caídos s/n, 37008 Salamanca, Spain.
Food Chem. 2015 May 1;174:348-55. doi: 10.1016/j.foodchem.2014.11.051. Epub 2014 Nov 14.
A simple, efficient and green analytical method for the determination of free nucleotide monophosphates in human milk is proposed. It involves centrifugal ultrafiltration (CUF) as sample treatment and capillary electrophoresis-electrospray mass spectrometry (CE-ESI-MS) for separation and simultaneous quantification. The optimised method, applied to the analysis of human milk samples, included their dilution (1:5) with water followed by CUF treatment. No matrix effects were found. The method provided limits of detection between 0.08 and 0.13 μg mL(-1) and limits of quantification between 0.26 and 0.43 μg mL(-1). The intralaboratory repeatability and reproducibility afforded relative standard deviation values lower than 10%. The method was applied to the study of the effects of Holder pasteurisation and high-pressure processing on the nucleotide contents in samples from a human milk bank. The results showed concentration values between 0.5 and 10 μg mL(-1), with higher concentrations for the samples treated by pasteurisation. The effect of freezing time on the content of nucleotides was also assessed.
提出了一种简单、高效、绿色的分析方法，用于测定人乳中的游离核苷酸单磷酸盐。它涉及离心超滤（CUF）作为样品处理，以及毛细管电泳-电喷雾质谱（CE-ESI-MS）用于分离和同时定量。该优化方法应用于人乳样品的分析，包括用去离子水稀释（1:5），然后进行 CUF 处理。未发现基质效应。该方法的检测限在 0.08 至 0.13μg/mL 之间，定量限在 0.26 至 0.43μg/mL 之间。实验室内部重复性和再现性提供的相对标准偏差值低于 10%。该方法应用于研究Holder 巴氏消毒法和高压处理对人乳库样品中核苷酸含量的影响。结果表明，浓度值在 0.5 至 10μg/mL 之间，巴氏消毒处理的样品浓度较高。还评估了冷冻时间对核苷酸含量的影响。
