title: Capillary electrophoresis fingerprinting of 8-aminopyrene-1,3,6-trisulfonate derivatized nitrocellulose after partial acid depolymerization.
abstract: Fine characterization of nitrocellulose (NC) remains a challenge, especially in forensic analysis, and a strategy consisting in obtaining representative fingerprints by a separation technique, as for proteins, is of prime interest. In this work, we first established that NCs (especially of high molar mass) cannot be representatively derivatized by 8-aminopyrene-1,3,6-trisulfonic acid (APTS), because of their poor solubility in the medium required for APTS derivatization. Therefore, a partial acid depolymerization step was considered, prior to derivatization by APTS, in an attempt to generate a mixture of oligosaccharides retaining information on the initial NC sample and/or on the cellulose used to prepare it. Acid depolymerization conditions (time and acid concentration) as well as APTS derivatization conditions (time, temperature, APTS/NC and reducing agent/APTS molar ratios) were investigated for lowly-nitrated NCs. The best compromise between depolymerization yields, speed, and pertinency of the resulting oligosaccharidic mixture was obtained using fuming hydrochloric acid (37%, w/w) at 50 °C for 30 min. The most effective procedure for APTS derivatization of oligosaccharides obtained after partial acid depolymerization of NC was achieved at 70 °C for 2h. The resulting APTS-derivatized oligosaccharides were then separated by capillary electrophoresis (CE) using a background electrolyte composed of 60mM 6-aminocaproic acid, pH 4.5 (adjusted with acetic acid)+0.02% hydroxypropyl methyl cellulose. Finally, for the first time, they were identified using APTS-derivatized cellodextrin standards and by matrix-assisted laser desorption-ionization time-of-flight mass spectrometry (MALDI-TOF MS).
authors.affiliation: PSL Research University, ESPCI ParisTech, LSABM, 10 rue Vauquelin, 75005 Paris, France; Central Laboratory of Police Prefecture (LCPP), 39bis rue de Dantzig, 75015 Paris, France; CNRS, CBI, UMR 8231, 10 rue Vauquelin, 75005 Paris, France.
authors.forename: Elodie
authors.initials: E
authors.lastname: Alinat
authors.affiliation: PSL Research University, ESPCI ParisTech, LSABM, 10 rue Vauquelin, 75005 Paris, France; CNRS, CBI, UMR 8231, 10 rue Vauquelin, 75005 Paris, France.
authors.forename: Nathalie
authors.initials: N
authors.lastname: Delaunay
authors.affiliation: Université Evry-Val-d'Essonne, Laboratoire Analyse et Modélisation pour la Biologie et l'Environnement, F-91025 Evry, France; CNRS, UMR 8587, Laboratoire Analyse et Modélisation pour la Biologie et l'Environnement, F-91025 Evry France.
authors.forename: Cédric
authors.initials: C
authors.lastname: Przybylski
authors.affiliation: Université Evry-Val-d'Essonne, Laboratoire Analyse et Modélisation pour la Biologie et l'Environnement, F-91025 Evry, France; CNRS, UMR 8587, Laboratoire Analyse et Modélisation pour la Biologie et l'Environnement, F-91025 Evry France.
authors.forename: Régis
authors.initials: R
authors.lastname: Daniel
authors.affiliation: Central Laboratory of Police Prefecture (LCPP), 39bis rue de Dantzig, 75015 Paris, France.
authors.forename: Xavier
authors.initials: X
authors.lastname: Archer
authors.affiliation: PSL Research University, ESPCI ParisTech, LSABM, 10 rue Vauquelin, 75005 Paris, France; CNRS, CBI, UMR 8231, 10 rue Vauquelin, 75005 Paris, France; PSL Research University, Chimie ParisTech, 11 rue Pierre et Marie Curie, 75005 Paris, France. Electronic address: pierre.gareil@chimie-paristech.fr.
authors.forename: Pierre
authors.initials: P
authors.lastname: Gareil
mesh_terms: D003101:Collodion / Q000032:analysis / Q000737:chemistry*; D019075:Electrophoresis, Capillary; D009844:Oligosaccharides / Q000737:chemistry; D011721:Pyrenes / Q000032:analysis*; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization
chemical_list: C103430:8-aminopyrene-1,3,6-trisulfonic acid; D009844:Oligosaccharides; D011721:Pyrenes; D003101:Collodion
keywords: 8-aminopyrene-1,3,6-trisulfonic acid; Acid hydrolysis.; Capillary electrophoresis; Fluorescence detection; Nitrocellulose fingerprints