In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GCQqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simplederivatization reaction with propyl chloroformate and pyridine carried out directly in water samples,followed by automated SPME analysis in the same vial without further sample handling. The affinity ofthe different derivatized compounds obtained towardsfive commercially available SPME coatings wasevaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GCQqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed theachievement of high specificity by selecting appropriate precursor–product ion couples improving thecapability in analyte identification. The multivariate approach of experimental design was crucial inorder to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters.Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L1, provided satisfactory values (114.2%,83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%,7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L1 were obtained. Thereliable application of the proposed protocol to real drinking water samples confirmed its capability to beused as analytical tool for routine analyses.

In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GC-QqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simple derivatization reaction with propyl chloroformate and pyridine carried out directly in water samples, followed by automated SPME analysis in the same vial without further sample handling. The affinity of the different derivatized compounds obtained towards five commercially available SPME coatings was evaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GC-QqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed the achievement of high specificity by selecting appropriate precursor-product ion couples improving the capability in analyte identification. The multivariate approach of experimental design was crucial in order to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters. Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L-1, provided satisfactory values (114.2%, 83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%, 7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L-1 were obtained. The reliable application of the proposed protocol to real drinking water samples confirmed its capability to be used as analytical tool for routine analyses. (C) 2014 Elsevier B.V. All rights reserved. OI Gionfriddo, Emanuela/0000-0002-1836-1950; sindona, giovanni/0000-0002-5623-5795; NACCARATO, Attilio/0000-0001-5799-5369; Tagarelli, Antonio/0000-0002-8811-1631

Determination of hydrazine in drinking water: development and multivariate optimization of a rapid and simple solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry protocol

Naccarato A;SINDONA, Giovanni;TAGARELLI, Antonio
2014

Abstract

In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GC-QqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simple derivatization reaction with propyl chloroformate and pyridine carried out directly in water samples, followed by automated SPME analysis in the same vial without further sample handling. The affinity of the different derivatized compounds obtained towards five commercially available SPME coatings was evaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GC-QqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed the achievement of high specificity by selecting appropriate precursor-product ion couples improving the capability in analyte identification. The multivariate approach of experimental design was crucial in order to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters. Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L-1, provided satisfactory values (114.2%, 83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%, 7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L-1 were obtained. The reliable application of the proposed protocol to real drinking water samples confirmed its capability to be used as analytical tool for routine analyses. (C) 2014 Elsevier B.V. All rights reserved. OI Gionfriddo, Emanuela/0000-0002-1836-1950; sindona, giovanni/0000-0002-5623-5795; NACCARATO, Attilio/0000-0001-5799-5369; Tagarelli, Antonio/0000-0002-8811-1631
In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GCQqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simplederivatization reaction with propyl chloroformate and pyridine carried out directly in water samples,followed by automated SPME analysis in the same vial without further sample handling. The affinity ofthe different derivatized compounds obtained towardsfive commercially available SPME coatings wasevaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GCQqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed theachievement of high specificity by selecting appropriate precursor–product ion couples improving thecapability in analyte identification. The multivariate approach of experimental design was crucial inorder to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters.Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L1, provided satisfactory values (114.2%,83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%,7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L1 were obtained. Thereliable application of the proposed protocol to real drinking water samples confirmed its capability to beused as analytical tool for routine analyses.
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/20.500.11770/134421
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