title: 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.
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.
authors: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via Pietro Bucci Cubo 12/C, Arcavacata di Rende (CS) I-87030, Italy.
authors: Emanuela
authors: E
authors: Gionfriddo
authors: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via Pietro Bucci Cubo 12/C, Arcavacata di Rende (CS) I-87030, Italy. Electronic address: attilio.naccarato@unical.it.
authors: Attilio
authors: A
authors: Naccarato
authors: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via Pietro Bucci Cubo 12/C, Arcavacata di Rende (CS) I-87030, Italy.
authors: Giovanni
authors: G
authors: Sindona
authors: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via Pietro Bucci Cubo 12/C, Arcavacata di Rende (CS) I-87030, Italy. Electronic address: a.tagarelli@unical.it.
authors: Antonio
authors: A
authors: Tagarelli
mesh_terms: D060766:Drinking Water / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006834:Hydrazines / Q000032:analysis*; D015999:Multivariate Analysis; D052617:Solid Phase Microextraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D060766:Drinking Water; D006834:Hydrazines; D014874:Water Pollutants, Chemical; C029424:hydrazine
keywords: Chloroformates; Drinking water; Experimental design; Gas chromatography; Hydrazine; Solid phase microextraction