Off‐line capillary electrophoresis/matrix‐assisted laser desorption/ionization tandem time‐of‐flight mass spectrometry for analysis of synthesized poly(amido)amine dendrimers

Glycine-modified polyamidoamine dendrimers: synthesis and structural characterization using nuclear magnetic resonance, ion-mobility mass spectrometry and capillary electrophoresis

“…1A-C, respectively) show multiple peaks between 2.35 and 3.50 ppm which correspond to the methylene protons of PAMAM branching units (the 1 H NMR spectrum of the unmodied PAMAM G1(N) exclusively displayed these peaks). These signals were assigned by a standard procedure including two dimensional 1 H-1 H homonuclear scalar correlation (COSY) 18 and 1 H- 13 C heteronuclear correlation (HMQC and HMBC). 19 Characteristic spin systems were rst identied in each structure from 1 H-1 H COSY and 1 H- 13 C HMQC NMR spectra.…”

“…8 On the other hand, unmodied small generation PAMAM dendrimers have been extensively studied by infra-red, ultra-violet/visible, nuclear magnetic resonance (NMR) and mass spectrometry (MS) techniques. [9][10][11][12][13] In particular, MS appeared to be useful for the full-characterization of small generation PAMAM dendrimers using either electrospray (ESI) or matrix assisted laser desorption ionization (MALDI) techniques. [10][11][12][13] To understand the molecular mechanisms involved in DNA/ modied-PAMAM complexes formation, the study of non covalent interactions implicated in such dendriplexes formation can be envisaged on small dendrimer models.…”

“…[9][10][11][12][13] In particular, MS appeared to be useful for the full-characterization of small generation PAMAM dendrimers using either electrospray (ESI) or matrix assisted laser desorption ionization (MALDI) techniques. [10][11][12][13] To understand the molecular mechanisms involved in DNA/ modied-PAMAM complexes formation, the study of non covalent interactions implicated in such dendriplexes formation can be envisaged on small dendrimer models. Thus, even if small generations of PAMAM are not expected to be applied in biomedical applications, we intend to design amino acid-modied G1 PAMAM as a good starting point for optimization and monitoring of the chemical design as well as for analytical methodology implementation.…”

“…CE and IM-MS were proposed as alternative techniques for cationic PAMAM separation, appending literature data. 13,14 Moreover, IM-MS is well-known to present the advantage to permit in a single run the separation and the identication of ionic species in the millisecond time-scale from direct infusion of samples (a prior LC separation being not necessarily required). It is the rst time to our knowledge that such comprehensive structural analysis is reported.…”

Capillary electrophoresis and nanomaterials – Part I: Capillary electrophoresis of nanomaterials

“…Polyamidoamine (PAMAM) dendrimers can be separated reasonably well at acidic pH but not at neutral pH. This point was considered in a number of papers directed towards the isolation and characterization of dendrimers . To improve run‐to‐run reproducibility, a silanized capillary was used , and monitoring of the removal of excess succinic anhydride/succinic acid enabled more detailed characterization of PAMAM samples .…”