Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method

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 ma...

Full description

Saved in:
Bibliographic Details
Main Authors: Beatriz Antunes, Andreia Videira, Ana Penetra, Vitor V. Cardoso, Rui N. Carneiro, Cristina M. M. Almeida
Format: Article
Language:English
Published: MDPI AG 2025-05-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/30/11/2403
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1849721797112496128
author Beatriz Antunes
Andreia Videira
Ana Penetra
Vitor V. Cardoso
Rui N. Carneiro
Cristina M. M. Almeida
author_facet Beatriz Antunes
Andreia Videira
Ana Penetra
Vitor V. Cardoso
Rui N. Carneiro
Cristina M. M. Almeida
author_sort Beatriz Antunes
collection DOAJ
description 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<sup>2</sup>) 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.
format Article
id doaj-art-5d4ee4675e344685a1cea4d4d441d77e
institution DOAJ
issn 1420-3049
language English
publishDate 2025-05-01
publisher MDPI AG
record_format Article
series Molecules
spelling doaj-art-5d4ee4675e344685a1cea4d4d441d77e2025-08-20T03:11:32ZengMDPI AGMolecules1420-30492025-05-013011240310.3390/molecules30112403Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS MethodBeatriz Antunes0Andreia Videira1Ana Penetra2Vitor V. Cardoso3Rui N. Carneiro4Cristina M. M. Almeida5iMed.UL, Faculdade de Farmácia, Universidade de Lisboa, 1649-003 Lisboa, PortugalDireção de Laboratórios, Empresa Portuguesa das Águas Livres, S.A.—EPAL, 800-003 Lisboa, PortugalDireção de Laboratórios, Empresa Portuguesa das Águas Livres, S.A.—EPAL, 800-003 Lisboa, PortugalDireção de Laboratórios, Empresa Portuguesa das Águas Livres, S.A.—EPAL, 800-003 Lisboa, PortugalDireção de Laboratórios, Empresa Portuguesa das Águas Livres, S.A.—EPAL, 800-003 Lisboa, PortugaliMed.UL, Faculdade de Farmácia, Universidade de Lisboa, 1649-003 Lisboa, PortugalNitrosamines (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<sup>2</sup>) 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.https://www.mdpi.com/1420-3049/30/11/2403GC-MSLLEmaterialsmigration assaysnitrosamineswater
spellingShingle Beatriz Antunes
Andreia Videira
Ana Penetra
Vitor V. Cardoso
Rui N. Carneiro
Cristina M. M. Almeida
Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
Molecules
GC-MS
LLE
materials
migration assays
nitrosamines
water
title Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
title_full Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
title_fullStr Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
title_full_unstemmed Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
title_short Assessing Nitrosamine Migration from Drinking Water Contact Materials Using a Validated LLE-GC-MS Method
title_sort assessing nitrosamine migration from drinking water contact materials using a validated lle gc ms method
topic GC-MS
LLE
materials
migration assays
nitrosamines
water
url https://www.mdpi.com/1420-3049/30/11/2403
work_keys_str_mv AT beatrizantunes assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod
AT andreiavideira assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod
AT anapenetra assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod
AT vitorvcardoso assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod
AT ruincarneiro assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod
AT cristinammalmeida assessingnitrosaminemigrationfromdrinkingwatercontactmaterialsusingavalidatedllegcmsmethod