Development of a method for the simultaneous determination of phosphoric and amino acid group containing pesticides by gas chromatography with mass-selective detection - Optimization of the derivatization procedure using an experimental design approach
Φόρτωση...
Ημερομηνία
Συγγραφείς
Stalikas, C. D.
Pilidis, G. A.
Τίτλος Εφημερίδας
Περιοδικό ISSN
Τίτλος τόμου
Εκδότης
Elsevier
Περίληψη
Τύπος
Είδος δημοσίευσης σε συνέδριο
Είδος περιοδικού
peer reviewed
Είδος εκπαιδευτικού υλικού
Όνομα συνεδρίου
Όνομα περιοδικού
Journal of Chromatography A
Όνομα βιβλίου
Σειρά βιβλίου
Έκδοση βιβλίου
Συμπληρωματικός/δευτερεύων τίτλος
Περιγραφή
An integrated gas chromatographic-mass-selective detection method for the analysis of the phosphoric and amino acid group containing pesticides is presented. The analytes are derivatized using a single-step procedure for the simultaneous esterification and acetylation of the active groups of analytes (-OH, -COOH, -NH2) by means of acetic acid and trimethyl orthoacetate. An experimental design approach based on the central composite design is used to investigate the dependence of the derivatization variables with the total yield of derivatization of pesticides. The variables selected for study were: the amount of reagents, the temperature and the reaction time. When considering the total pesticide derivatization yield, the amount of acetic acid, the reaction temperature and the reaction time are found to be statistically significant. The electron impact ionization mass spectra of the resulting derivatives are acquired and properly interpreted. Under the chromatographic conditions employed, acceptable peak separation is attained. When the selective ion monitoring mode is used for quantitation purposes, low detection limits in the range 0.05 to 14 mu g/l are achieved. Recoveries of spiked water samples range from 96 to 103% and the mean RSD of the method do not exceed 3.5%. (C) 2000 Elsevier Science B.V. All rights reserved.
Περιγραφή
Λέξεις-κλειδιά
experimental design, central composite design, chemometrics, derivatization, gc, method development, optimization, pesticides, organophosphorus compounds, column liquid-chromatography, (aminomethyl)phosphonic acid, aminomethylphosphonic acid, herbicides glyphosate, rapid-determination, glufosinate, water, samples, residues, simplex
Θεματική κατηγορία
Παραπομπή
Σύνδεσμος
<Go to ISI>://000085807800017
http://ac.els-cdn.com/S002196739901300X/1-s2.0-S002196739901300X-main.pdf?_tid=6eaa477d8d75ea426e42148a7941aeaa&acdnat=1333041025_fea3b64b9d0257dcbbdb440748d1eb78
http://ac.els-cdn.com/S002196739901300X/1-s2.0-S002196739901300X-main.pdf?_tid=6eaa477d8d75ea426e42148a7941aeaa&acdnat=1333041025_fea3b64b9d0257dcbbdb440748d1eb78
Γλώσσα
en
Εκδίδον τμήμα/τομέας
Όνομα επιβλέποντος
Εξεταστική επιτροπή
Γενική Περιγραφή / Σχόλια
Ίδρυμα και Σχολή/Τμήμα του υποβάλλοντος
Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας