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高效液相色谱-三重四极杆质谱法测定抗坏血酸及其降解产物。

Determination of ascorbic acid and its degradation products by high-performance liquid chromatography-triple quadrupole mass spectrometry.

机构信息

Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, Torun, Poland.

出版信息

Electrophoresis. 2014 Feb;35(4):585-92. doi: 10.1002/elps.201300439. Epub 2014 Jan 13.

DOI:10.1002/elps.201300439
PMID:24469997
Abstract

This study describes application of liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS) for evaluation of vitamin C stability, the objective being prediction of the degradation products. Detection was performed with an UV detector (UV-Vis) in sequence with a triple-quad mass spectrometer in the multiple reaction mode. The negative ion mode of ESI and MS-MRM transitions of m/z 175→115 (quantifier) and 175→89 (qualifier) for ascorbic acid was used. All the validation parameters were within the range of acceptance proposed by the Food and Drug Administration. The method was fully validated in terms of linearity, LOD, LOQ, accuracy, and interday precision. Validation experiments revealed good linearity with R(2) = 0.999 within the established concentration range, and excellent repeatability (9.3%). The LOD of the method was 0.1524 ng/mL whereas the LOQ was 0.4679 ng/mL. LC-MS methodology proves to be an improved, simple, and fast approach to determining the content of vitamin C and its degradation products with high sensitivity, selectivity, and resolving power within 6 minutes of analysis.

摘要

本研究描述了液相色谱-串联三重四极杆质谱(LC-MS)在维生素 C 稳定性评估中的应用,旨在预测降解产物。检测采用紫外检测器(UV-Vis)依次与三重四极杆质谱在多反应模式下进行。ESI 的负离子模式和 MS-MRM 跃迁 m/z 175→115(定量器)和 175→89(定性器)用于抗坏血酸。所有验证参数均在食品和药物管理局提出的可接受范围内。该方法在线性、LOD、LOQ、准确度和日间精密度方面进行了全面验证。验证实验表明,在建立的浓度范围内,具有良好的线性关系,R(2) = 0.999,且重复性极好(9.3%)。该方法的 LOD 为 0.1524ng/mL,LOQ 为 0.4679ng/mL。LC-MS 方法被证明是一种改进的、简单的、快速的方法,可在 6 分钟的分析时间内实现高灵敏度、选择性和分辨率,用于测定维生素 C 及其降解产物的含量。

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