APCI/APPI for synthetic polymer analysis

Terrier, Péran; Desmazières, Bernard; Tortajada, Jeanine; Buchmann, William

doi:10.1002/mas.20302

Cited by 51 publications

(45 citation statements)

References 99 publications

(123 reference statements)

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“…24,25 In this case only negative ions, M − , were recorded in an appropriate mass range at 70 000 mass resolution. The APCI probe was used without a flow of solvent, although a solution of reserpine was introduced through the APCI probe during the experiments to serve as a lock mass in negative ion mode.…”

Section: Mass Spectrometrymentioning

confidence: 99%

Characterization of the prepolymer and gel of biocompatible poly(xylitol sebacate) in comparison with poly(glycerol sebacate) using a combination of mass spectrometry and nuclear magnetic resonance

Moorhoff

Cook

et al. 2014

Polymer International

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Atmospheric pressure chemical ionization (negative ion) and electrospray ionization (positive and negative ion) mass spectrometry and nuclear magnetic resonance ( 1 H NMR and 13 C NMR) were used to characterize the prepolymer (i.e. uncrosslinked) poly(xylitol sebacate) (PXS), prepared by condensation of xylitol [X] and sebacic acid [S], and this was compared with poly(glycerol sebacate) (PGS), prepared by condensation of glycerol [G] and [S]. The PXS prepolymer, prepared at 118 ∘ C/24 h, gave predominantly 1-acyl-[XS] and 1,5-diacyl-[SXS] species and smaller amounts of 2-acyl substitutions. At 130 ∘ C/24 h an increase of the amount of the 1-acyl and 1,5-diacyl substitutions in the [(SX) n ], [S(XS) n ] and [(XS) n X] series was identified, as was found for the analogous PGS prepolymer ([(SG) n ], [S(GS) n ] and [(GS) n G] series). Novel tetrahydrofuranyl species were found in the PXS prepolymer. Further polymerization of the PXS prepolymer gave a gel which when analysed using 13 C NMR was shown to mainly contain 1-acyl and 1,5-diacyl substitutions.

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Section: Mass Spectrometrymentioning

confidence: 99%

Characterization of the prepolymer and gel of biocompatible poly(xylitol sebacate) in comparison with poly(glycerol sebacate) using a combination of mass spectrometry and nuclear magnetic resonance

Moorhoff

Cook

et al. 2014

Polymer International

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“…Unbelievably, at first glance, the O-protonated p-DMABA could be produced by APCI. In APCI, the sample solution first evaporates to form a gaseous state, and then the analyte ions are formed through corona discharge and ion/molecule reactions; thus, it seems reasonable that the gas-phase thermodynamically favored ion should be formed [41][42][43]. The CID spectra of the [M + H] + ion of p-DMABA generated by APCI from different solvents exhibit clear difference, as shown in Figure 2.…”

Section: Protonation Site In Atmospheric Pressure Chemical Ionizationmentioning

confidence: 99%

The Protonation Site of para-Dimethylaminobenzoic Acid Using Atmospheric Pressure Ionization Methods

Chai

Weng

Shen

et al. 2015

J. Am. Soc. Mass Spectrom.

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Abstract. The protonation site of para-dimethylaminobenzoic acid (p-DMABA) was investigated using atmospheric pressure ionization methods (ESI and APCI) coupled with collision-induced dissociation (CID), nuclear magnetic resonance (NMR), and computational chemistry. Theoretical calculations and NMR experiments indicate that the dimethyl amino group is the preferred site of protonation both in the gas phase and aqueous solution. Protonation of p-DMABA occurs at the nitrogen atom by ESI independent of the solvents and other operation conditions under typical thermodynamic control. However, APCI produces a mixture of the nitrogen-and carbonyl oxygenprotonated p-DMABA when aprotic organic solvents (acetonitrile, acetone, and tetrahydrofuran) are used, exhibiting evident kinetic characteristics of protonation. But using protic organic solvents (methanol, ethanol, and isopropanol) in APCI still leads to the formation of thermodynamically stable N-protonated p-DMABA. These structural assignments were based on the different CID behavior of the N-and O-protonated p-DMABA. The losses of methyl radical and water are the diagnostic fragmentations of the N-and O-protonated p-DMABA, respectively. In addition, the N-protonated p-DMABA is more stable than the O-protonated p-DMABA in CID revealed by energy resolved experiments and theoretical calculations.

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“…A recent paper reviews the use of APCI and the closely related atmospheric-pressure photoionization (APPI) technique in the characterization of synthetic polymers [294]. Next to protonation, the formation of [M + Na] + -ions is important in APCI-MS analysis of synthetic polymers.…”

Section: Synthetic Polymersmentioning

confidence: 99%

Ion/Molecule Attachment Reactions: Mass Spectrometry

Fujii¹

2015

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APCI/APPI for synthetic polymer analysis

Cited by 51 publications

References 99 publications

Characterization of the prepolymer and gel of biocompatible poly(xylitol sebacate) in comparison with poly(glycerol sebacate) using a combination of mass spectrometry and nuclear magnetic resonance

Characterization of the prepolymer and gel of biocompatible poly(xylitol sebacate) in comparison with poly(glycerol sebacate) using a combination of mass spectrometry and nuclear magnetic resonance

The Protonation Site of para-Dimethylaminobenzoic Acid Using Atmospheric Pressure Ionization Methods

Ion/Molecule Attachment Reactions: Mass Spectrometry

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