Pérez-Ruiz Tomás, Martínez-Lozano Carmen, Tomás Virginia, Martín Jesús
Department of Analytical Chemistry, Faculty of Chemistry University of Murcia, 30071 Murcia, Spain.
J Chromatogr A. 2004 Feb 13;1026(1-2):57-64. doi: 10.1016/j.chroma.2003.10.130.
An HPLC method was developed for the determination of citric, lactic, malic, oxalic and tartaric acids by chemiluminescent detection following online irradiation with visible light. The organic acids were irradiated with visible light in the presence of Fe3+ and UO2(2+) to generate Fe2+, which was determined by measuring the chemiluminescence intensity in a luminol system in the absence of added oxidant. Factors affecting the photochemical and chemiluminescence reactions were optimised so that their contribution to the total band-broadening was negligible. The chromatographic separation was performed on a C18 column under isocratic reversed-phase conditions using 0.005 M H2SO4 mobile phase. The optimised method was validated with respect to linearity, precision, limits of detection and quantification, accuracy specificity and robustness. The applicability of the assay was demonstrated by analysing these compounds in real samples such as milk, fruit juices, soft drinks, wine and beer.
建立了一种高效液相色谱法，用于测定柠檬酸、乳酸、苹果酸、草酸和酒石酸。该方法通过在线可见光照射后进行化学发光检测。有机酸在Fe3+和UO2(2+)存在下用可见光照射以生成Fe2+，通过在不添加氧化剂的鲁米诺体系中测量化学发光强度来测定Fe2+。对影响光化学和化学发光反应的因素进行了优化，使其对总谱带展宽的贡献可忽略不计。色谱分离在C18柱上进行，采用等度反相条件，流动相为0.005 M H2SO4。该优化方法在线性、精密度、检测限和定量限、准确度、特异性和稳健性方面进行了验证。通过分析牛奶、果汁、软饮料、葡萄酒和啤酒等实际样品中的这些化合物，证明了该测定方法的适用性。
