Characterization of synthetic polymers by MALDI-MS

Montaudo, Giorgio; Samperi, Filippo; Montaudo, Maurizio S.

doi:10.1016/j.progpolymsci.2005.12.001

Cited by 408 publications

(335 citation statements)

References 417 publications

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“…The use of ion-exchange beads (IXB) benefited the analysis, while the addition of sodium acetate (NaOAc A lthough matrix-assisted laser desorption/ ionization time-of-flight mass spectrometry (MALDI-TOFMS) has been utilized predominately within the life sciences, there has been considerable use of this technique for the characterization of synthetic polymers. The large body of work in this area has been the subject of several reviews [1][2][3]. However, there are few examples of the characterization of poly(methacrylic acid) (PMAA) homopolymers by MALDI-TOFMS in the literature.…”

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confidence: 99%

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Strategies for the analysis of poly(methacrylic acid) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

Wyatt

Schaeffer

Tan

et al. 2007

J. Am. Soc. Mass Spectrom.

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We evaluated several aqueous-based sample preparation protocols for the analysis of poly(methacrylic acid) (PMAA) by matrix-assisted laser desorption/ionization time-offlight mass spectrometry (MALDI-TOFMS). The sample contained a pentaerythritol tetra(3-mercaptopropionate) end-group, and was characterized in positive and negative ion modes using 2,5-dihydroxybenzoic acid (DHB) and 2,4,6-trihydroxyacetophenone (THAP) matrices. The major series observed were the [M ϩ Na] ϩ species, in positive ion mode, and the [M Ϫ H] Ϫ species, in negative ion mode. The performance of DHB and THAP matrices was comparable in positive ion mode, but THAP outperformed DHB in negative ion mode. The use of ion-exchange beads (IXB) benefited the analysis, while the addition of sodium acetate (NaOAc A lthough matrix-assisted laser desorption/ ionization time-of-flight mass spectrometry (MALDI-TOFMS) has been utilized predominately within the life sciences, there has been considerable use of this technique for the characterization of synthetic polymers. The large body of work in this area has been the subject of several reviews [1][2][3]. However, there are few examples of the characterization of poly(methacrylic acid) (PMAA) homopolymers by MALDI-TOFMS in the literature. The analytical protocols used in positive ion mode are 2,5-dihydroxybenzoic acid (DHB) matrix in methanol [4] or DHB and sodium trifluoroacetate in acetone [5]. Sinapinic acid in methanol (MeOH) or water (H 2 O) has been used in negative ion mode [6]. Consistent throughout these data are very poor signal-to-noise ratios and non-isotopic resolution of the observed species.The current investigation is concerned with the analysis of a low molecular weight PMAA sample containing a pentaerythritol tetra(3-mercaptopropionate) end group (PTMP-PMAA), shown in Figure 1, by MALDI-TOFMS. This polymer and similar ligands have been used as a ligand in the size-controlled synthesis of gold nanoparticles, which are only soluble in water [7,8]. The goal of the study was to establish aqueous-based sample preparation protocols that would provide data with improved signal-to-noise ratios and resolution compared with existing methods. These protocols could subsequently be used for the characterization of the PMAA-coated gold nanoparticles [8]. ExperimentalDHB and 2,4,6-trihydroxyacetophenone (THAP) matrices, and trifluoroacetic acid (TFA), were purchased from Fluka (Dorset, UK). Dowex 50W-X8, 200 m, ion-exchange beads (IXB), di-ammonium hydrogen citrate (DAC), sodium acetate (NaOAc), and ammonium acetate were purchased from Sigma-Aldrich (Dorset, UK). IXB were loaded with NH 4 ϩ ions as reported previously [9]. HPLC grade acetonitrile (MeCN) and MeOH, both purchased from Fisher Scientific (Loughborough, UK), and Milli-Q H 2 O (Watford, UK) were used where appropriate. PTMP-PMAA (M n ϭ 1900 g mol Ϫ1 and M w ϭ 2240 g mol Ϫ1 by GPC) was synthesized as reported elsewhere [8].DHB and THAP matrix solutions were made to a concentration of 10 mg mL Ϫ1 in 1:1 (vol/vol) H 2 O/ MeCN. DHB solution wa...

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mentioning

confidence: 99%

“…The large body of work in this area has been the subject of several reviews [1][2][3]. However, there are few examples of the characterization of poly(methacrylic acid) (PMAA) homopolymers by MALDI-TOFMS in the literature.…”

mentioning

confidence: 99%

Strategies for the analysis of poly(methacrylic acid) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

Wyatt

Schaeffer

Tan

et al. 2007

J. Am. Soc. Mass Spectrom.

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“…In particular, MALDI-MS offers an easy, robust, versatile, sensitive, and tolerant sample introduction tool for analysis of peptides, 6,7 proteins, 8,9 oligonucleotides, 10 DNA, 11 polymers, [12][13][14] small molecules, 15,16 and so on. With the goal of optimizing MALDI-MS analysis, extensive efforts have been made to investigate matrix effect, 17,18 matrix additives, 19 sample-matrix preparation methods, [20][21][22] and its mechanism.…”

Section: Introductionmentioning

confidence: 99%

“…MALDI-TOF MS analysis of synthetic polymers readily provides polymer characteristic information such as the average molar mass (M W ), molar mass distribution (MMD), repeat unit structure, copolymer sequence, and the endgroup. 12 Since MALDI mass spectra of synthetic polymers are sensitive to a variety of factors such as the matrix, mixing ratios of matrix/polymer/cationization agent, and the sample preparation method, careful selection of such experimental factors is needed. For example, the matrices commonly used in the analysis of polymers are a little different from those used for peptides, and the optimal matrices for specific polymers are well documented.…”

Section: Introductionmentioning

confidence: 99%

MALDI-TOF Analysis of Polyhexamethylene Guanidine (PHMG) Oligomers Used as a Commercial Antibacterial Humidifier Disinfectant

Hwang

Nam

Yang

et al. 2013

Bulletin of the Korean Chemical Society

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Polyhexamethylene guanidine (PHMG) polymers used as an active ingredient in an antibacterial humidifier disinfectant were reported to cause harm to the human health when inhaled, although physical contact with this material was known to present low toxicity to humans. It is therefore necessary to develop an optimal analysis method which enables detection and analysis of PHMG polymers. MALDI-TOF investigations of PHMG are performed with a variety of matrices, and it is found that CHCA and 2,5-DHB are excellent matrices which well reflects the polymer population even at high mass. For the provided PHMG sample, the number-average (M n ) and weight-average (M w ) molecular masses were determined to be 744.8 and 810.7, respectively, when the CHCA was used as a matrix. The rank of the matrices in terms of averaged molecular weight was CHCÃ 2,5-DHB > 5-NSA > DHAP, THAP > ATT > IAA ~ super-DHB ~ HABA. In addition, PSD of the PHMG oligomer ions exhibited a few unique fragmenation characteristics. The formation of a-and c-type fragments was the major fragmentation pathway, and the 25-Da loss peaks generally accompanied a-and c-type fragments.

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“…[1][2][3][4][5] However, MALDI mass spectra only provide information pertaining to molecular-weight, such as protonated, deprotonated or cationized molecules. In an effort to overcome this limitation, tandem mass spectrometry (collision-induced dissociation, CID, or post source decay) has been employed to provide some additional structural information.…”

Section: Introductionmentioning

confidence: 99%

A Novel Derivatization Reagent in the Determination of the Number of OH End Groups in Poly(ethylene glycol) by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

Kagawa

2013

Mass Spectrometry

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The potential of a novel derivatization reagent, trifluoroacetic anhydride (TFAA), in determining the number of OH groups in poly(ethylene glycol) (PEG) was investigated by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). The MALDI mass spectra of the products revealed peaks of sodiated derivative cations, whose shift by the respective increments, ∆m/z: 96 × number of OH, allowed for the determination of the number of end functional groups with active hydrogens. In the present study, complete acylation of OH groups by TFAA proceeded rapidly, and only required mixing in acetonitrile solvent without purification. As a result, the number of OH end groups of PEG could be determined rapidly.

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Characterization of synthetic polymers by MALDI-MS

Cited by 408 publications

References 417 publications

Strategies for the analysis of poly(methacrylic acid) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

Strategies for the analysis of poly(methacrylic acid) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

MALDI-TOF Analysis of Polyhexamethylene Guanidine (PHMG) Oligomers Used as a Commercial Antibacterial Humidifier Disinfectant

A Novel Derivatization Reagent in the Determination of the Number of OH End Groups in Poly(ethylene glycol) by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

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