title: Large volume injection of water in gas chromatography–mass spectrometry using the Through Oven Transfer Adsorption Desorption interface: Application to multiresidue analysis of pesticides.
abstract: In the present work, the potential of the Through Oven Transfer Adsorption Desorption (TOTAD) interface for the large volume injection (LVI) of aqueous samples in gas chromatography (GC) using a mass spectrometry (MS) detector is demonstrated. To this end, a new method for the determination of pesticides in water is presented, being the first developed method in which injection of large amounts of polar solvents using the TOTAD interface and an MS detector are combined, is applied to the determination of pesticides in water. Water samples, as large as 5 ml, were directly injected into a capillary GC. No sample pre-treatment step other than simple filtration was needed. The TOTAD interface allows the introduction of several millilitres of water, while maintaining good chromatographic characteristics. The water is almost entirely eliminated, so that LVI of aqueous samples and an MS detector can be used without problems. Organophosphorus, organochlorine, and triazine pesticides were determined in one run. Calibration curves were linear in the range tested and the sensitivity achieved injecting 5 ml of water sample was sufficient for most of the target pesticides but not for all of them. Sensitivity of the analysis can be improved by increasing the sample volume. No variability was observed in the retention times and relative standard deviations from absolute peak areas were good, considering that they corresponded to the overall analysis. The method was applied to the analysis of pesticide residues in real water samples.
authors.affiliation: Escuela Técnica Superior de Ingenieros Agrónomos, Universidad de Castilla-La Mancha, Campus Universitario, Albacete, Spain.
authors.forename: Rosa M
authors.initials: RM
authors.lastname: Toledano
authors.forename: Jose M
authors.initials: JM
authors.lastname: Cortés
authors.forename: Juan C
authors.initials: JC
authors.lastname: Andini
authors.forename: Jesús
authors.initials: J
authors.lastname: Villén
authors.forename: Ana
authors.initials: A
authors.lastname: Vázquez
mesh_terms: D000327:Adsorption; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D010573:Pesticide Residues; D014874:Water Pollutants, Chemical; D014867:Water