Tankiewicz Maciej, Olkowska Ewa, Berg Andrzej, Wolska Lidia
Department of Environmental Toxicology, Faculty of Health Sciences With Institute of Maritime and Tropical Medicine, Medical University of Gdansk, Gdansk, Poland.
Front Chem. 2020 Jan 15;7:928. doi: 10.3389/fchem.2019.00928. eCollection 2019.
A gas chromatography-mass spectrometry (GC-MS) method to determine polar and thermally unstable phthalate metabolites [monomethyl phthalate-MMP, monoethyl phthalate-MEP, mono--butyl phthalate-MnBP, mono-(2-ethylhexyl) phthalate-MEHP] has been developed. This is the first report presenting the separation of monophthalates without derivatization step and any additional equipment or special injection port. Injection parameters (temperature, pressure, time, and volume of injection), chromatographic separation (retention gap, temperature program), and MS detection/identification (working parameters, ion selection) were investigated. Mechanisms and phenomena occurring under different conditions in the GC injector were evaluated and discussed. The limits of detection (LODs) of MMP, MEP, MnBP, MEHP in the protocol were 0.049, 0.036, 0.038, and 0.029 ng ( 2 μL of injection), respectively. The response of the monophthalates was found to be linear in the tested concentration range (for MMP: 0.15-100 ng, MEP and MnBP: 0.11-100 ng, MEHP: 0.087-100 ng 2 μL) with the coefficient of determination higher than 0.9817 and inter-day precision in the range of 1.4-5.4%. The developed method is fast, easy and repeatable. Moreover, it allows for the elimination of derivatization agents, reduction of toxic waste production and simplification of analytical procedure.
已开发出一种气相色谱 - 质谱联用（GC - MS）方法，用于测定极性和热不稳定的邻苯二甲酸酯代谢物[单甲基邻苯二甲酸酯 - MMP、单乙基邻苯二甲酸酯 - MEP、单丁基邻苯二甲酸酯 - MnBP、单（2 - 乙基己基）邻苯二甲酸酯 - MEHP]。这是第一份报告，介绍了无需衍生化步骤以及任何额外设备或特殊进样口即可分离单邻苯二甲酸酯。研究了进样参数（温度、压力、时间和进样体积）、色谱分离（保留间隙、温度程序）以及质谱检测/鉴定（工作参数、离子选择）。对GC进样器在不同条件下发生的机制和现象进行了评估和讨论。该方法中MMP、MEP、MnBP、MEHP的检测限（LOD）分别为0.049、0.036、0.038和0.029 ng（进样2 μL）。发现单邻苯二甲酸酯在测试浓度范围内呈线性响应（对于MMP：0.15 - 100 ng，MEP和MnBP：0.11 - 100 ng，MEHP：0.087 - 100 ng / 2 μL），测定系数高于0.9817，日间精密度在1.4 - 5.4%范围内。所开发的方法快速、简便且可重复。此外，它无需使用衍生化试剂，减少了有毒废物的产生，并简化了分析程序。
