Antunes Beatriz, Videira Andreia, Penetra Ana, Cardoso Vitor V, Carneiro Rui N, Almeida Cristina M M
iMed.UL, Faculdade de Farmácia, Universidade de Lisboa, 1649-003 Lisboa, Portugal.
Direção de Laboratórios, Empresa Portuguesa das Águas Livres, S.A.-EPAL, 800-003 Lisboa, Portugal.
Molecules. 2025 May 30;30(11):2403. doi: 10.3390/molecules30112403.
Nitrosamines (NAs) are toxic compounds associated with disinfection processes. Human exposure can occur through the hydraulic hoses and seals that are in contact with drinking water. This study develops and validates a chromatographic method to quantify 11 NAs in water leachates from four organic materials. The method is based on liquid-liquid extraction (LLE) followed by gas chromatography coupled with mass spectrometry (GC-MS). The method was validated by the application of several statistical tests, namely, linearity/working range, precision, trueness, and recovery tests. The GC-MS method showed a good linear range for all NAs with coefficients of determination (r) higher than 0.9989, coefficients of variation of the method (CVm) lower than 2.5%, and PG < F (0.05; 1; N-3). The working range varies between 10 µg/L and 386.7 µg/L. The GC-MS method showed good precision under repeatability and reproducibility conditions with a relative standard deviation (RSD) lower than 12% and 10%, respectively. The GC-MS showed good trueness with a relative error lower than 20%. Matrix effects were significant, with recovery (Rec) values between 47% and 125% and an RSD lower than 20%. The limit of detection (LOD) and quantification (LOQ) ranged between 0.71 µg/L and 8.9 µg/L and between 2.3 µg/L and 29.8 µg/L, respectively. The method quantification limits (MQL) ranged from 0.0045 µg/L to 0.0378 µg/L. The sum of the MQL (0.2 µg/L) is lower than the reference limit of 0.3 µg/L for NAs in the leachates from the migration tests. Four organic materials were subjected to migration tests with demineralized and chlorinated water to assess their suitability for the water supply system. These materials met the NA specifications for use in the water network.
亚硝胺（NAs）是与消毒过程相关的有毒化合物。人类可通过与饮用水接触的液压软管和密封件接触到它们。本研究开发并验证了一种色谱方法，用于定量四种有机材料水浸出液中的11种亚硝胺。该方法基于液液萃取（LLE），随后进行气相色谱-质谱联用（GC-MS）。通过应用几种统计测试对该方法进行了验证，即线性/工作范围、精密度、准确性和回收率测试。GC-MS方法对所有亚硝胺均显示出良好的线性范围，测定系数（r）高于0.9989，方法变异系数（CVm）低于2.5%，且PG < F（0.05；1；N - 3）。工作范围在10 μg/L至386.7 μg/L之间。GC-MS方法在重复性和再现性条件下显示出良好的精密度，相对标准偏差（RSD）分别低于12%和10%。GC-MS显示出良好的准确性，相对误差低于20%。基质效应显著，回收率（Rec）值在47%至125%之间，RSD低于20%。检测限（LOD）和定量限（LOQ）分别在0.71 μg/L至8.9 μg/L和2.3 μg/L至29.8 μg/L之间。方法定量限（MQL）范围为0.0045 μg/L至0.0378 μg/L。MQL总和（0.2 μg/L）低于迁移试验浸出液中亚硝胺的参考限值0.3 μg/L。对四种有机材料进行了用软化水和加氯水的迁移试验，以评估它们在供水系统中的适用性。这些材料符合用于水网络的亚硝胺规格要求。
