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AminopropylheptakislisobutyDPOSS (P0SS-NH2, 97%) was purchased from Hybrid Plastics.
All experiments were performed on a Waters QToF2 mass spectrometer. The analyte solutions were delivered to the ESi source by a Harvard Apparatus syringe pump at a flow rate of 5μLmin-1. Typical ESI conditions were: capillary voltage, 3.1 kV; cone voltage, 15V; source temperature, 80°C; desolvation temperature, 120°C. Dry nitrogen was used as the ESI gas. For the recording of the single-stage ESI-MS spectra, the quadrupole (rf-only mode) was set to pass ions from 50Th to 1000Th, and all ions were transmitted into the pusher region of the time-of-flight analyzer where they were mass analyzed with 1 s integration time. Data were acquired in continuum mode until acceptable averaged data were obtained. For the ESI-MS/MS CID experiments, the ions of interest are mass-selected by the quadrupole mass filter. The precursor ion resolution is adjusted to select only the monoisotopic signal amongst the complete isotopic cluster. The selected ions are then submitted to collision against argon in the rf-only hexapole collision cell. All ions coming out of the hexapole cell, either the fragments or the non dissociated precursor ions, are finally mass-measured with the oa-ToF analyzer.
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R. Kaufmann, B. Spengler and F. Lutzenkirchen, "Mass-spectrometric sequencing of Linear peptides by product-ion analysis in a reflectron time-of-flight massspectrometer using matrix-assisted laser-desorption ionization", Rapid Commun. Mass Spectrom. 7, 702 (1993). doi: 10.1002/rcm. 1290071010
R. G. Cooks, J. H. Beynon, R. M. Caprioli and G. R. Lester, Metastable Ions. Elsevier Scientific Publishing Company, Amsterdam, The Netherlands (1973).
D. J. Harvey, A. P. Hunter, R. H. Bateman, J. Brown and G. Critchley, "Relationship between in-source and post-source fragment ions in the matrix-assisted laser desorption (ionization) mass spectra of carbohydrates recorded with reflectron time-of-flight mass spectrometers", Int. J. Mass Spectrom. 188, 131 (1999). doi: 10.1016/S1387-38061991000U-7
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In a glovebox, 0.06 g (nNH2=2.510-4 mol) of hexadecylamine and 0.36g (nl-A=2.510-3 mol) of dried L-lactide were introduced by the glove box in a previousely flamed and nitrogen purged two-neck flask equipped with a three-way stopcock and a magnetic stirring bar. Outside of the box, the L-lactide/hexadecylamine mixture was charged successively by toluene (4mL) and tin (II) octoate (Sn (Oct) 2; 1 mL of a 0.1 M toluene solution) under nitrogen by using previously flame-dried syringes. The mixture was then heated at 75°C under stirring. After 20 h, the polymerization was stopped by adding a few drops of diluted hydrochloric acid (1 M). The obtained polymer was then precipitated out from cold heptane, filtered and dried under vacuum at 40°C. 1H-NMR (300MHz, CDCl3, δ (ppm)): 0.8-1 (t, 3H), 1.3 (s, 28H), 1.5-1.9 (d, 3 (2n + 1) H), 3.8 (m, 2H), 4.4 (q, 1H; CH-OH), 5-5.3 (q, 2nH), 6.2 (1H; NH).
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G. Adamus, "Structural analysis of poly ((R, S)-3- hydroxybutyrate-co-L-lactide) copolyesters by electrospray ionization ion trap mass spectrometry", Rapid Commun. Mass Spectrom. 21, 2477 (2007). doi: 10.1002/rcm.3111
J. De Winter, 0. Coulembier, P. Marsal, J. Cornil, P. Dubois and P. Gerbaux, in preparation.
