scholarly journals Evaluation of the Degree of Polymerization of the Proanthocyanidins in Cranberry by Molecular Sieving and Characterization of the Low Molecular Weight Fractions by UHPLC-Orbitrap Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1504 ◽  
Author(s):  
Claudio Gardana ◽  
Paolo Simonetti
Keyword(s):  
Molecular Weight ◽  
Molecular Sieves ◽  
Degree Of Polymerization ◽  
Low Molecular Weight ◽  
Molecular Weight Distributions ◽  
Orbitrap Mass Spectrometry ◽  
Weight Distributions ◽  
Molecular Weight Fractions ◽  
Molecular Sieving

4-dimethylammino-cinnamaldehyde (DMAC) assays quantify total proanthocyanidins (PACs) but do not provide qualitative PAC molecular weight distribution information and cannot discriminate between A- and B-type PACs. We developed an efficient method for assessing PAC molecular weight distributions. The PACs from three commercial cranberry extracts (A1–A3) were fractionated by molecular sieves with cut-offs of 3, 10, 30, 50, and 100 kDa, and each fraction was analyzed by DMAC assays. A1, A2, and A3 contained 27%, 33%, and 15% PACs, respectively. Approximately 28 PACs, 20 flavonols, and 15 phenolic acids were identified by UHPLC-DAD-Orbitrap MS in A1 and A3, while A2 contained only flavan-3-ols. Epicatechin was the main monomer in A1 and A3, and catechin was the main in A2. Procyanidin A2 was the main dimer in A1 and A3, representing more than 85% of the total dimers, while it constituted approximately only 24% of A2. A1 and A3 contained quercetin, isorhamnetin, myricetin, and their glycosides, which were totally absent in A2. In A1 and A3 the PACs were mainly distributed in the fractions 30–3 and <3 kDa, while in A2 more than 70% were present in the fraction less than 3 kDa. Overall, obtained data strongly suggests that A2 is not cranberry-derived, or is adulterated with another source of PACs.

Characterization of Elution Chromatography Fractions from CIS-Polybutadiene by GPC

1970 ◽  
Vol 43 (6) ◽  
pp. 1439-1450 ◽  
Author(s):  
W. V. Smith ◽  
S. Thiruvengada
Keyword(s):  
Molecular Weight ◽  
Molecular Weight Distribution ◽  
Weight Distribution ◽  
Low Molecular Weight ◽  
Molecular Weight Distributions ◽  
Weight Distributions ◽  
Log Normal ◽  
Analytical Fractionation ◽  
Molecular Weight Fractions ◽  
Elution Chromatography

Abstract A preparative fractionation of about 23 g of a commercial cis-polybutadiene rubber is described. The method employed was a solvent elution chromatographic method with very little temperature gradient. The molecular weight distributions of the fractions obtained were determined by an analytical fractionation of 20 mg of polymer. The method was similar to the preparative fractionation and involved solvent elution chromatography. The fractions obtained were assayed for quantity, molecular weight, and molecular weight distribution by GPC. The low molecular weight fractions of the preparative fractionation had molecular weight distributions which could be closely approximated by two log normal distributions, the low molecular weight component having the narrower width. The ratio of weight to number average molecular weight was found to be about 1.1 for these samples. The higher molecular weight fractions could also be approximated by two log normal distributions; however, in these fractions the low molecular weight component had a very broad distribution but constituted only a small portion of the sample. The widths of the GPC curves of the fractions correlate satisfactorily with the molecular weight distributions found by the analytical refractionations. The GPC width is a sensitive criterion of the width of the molecular weight distribution even when only two columns are used. It is felt that the analytical fractionation procedure presented gives more detailed information on the molecular weight distribution than is easily obtainable from an ordinary GPC curve.

The Use of Novel F-RAFT Agents in High Temperature and High Pressure Ethene Polymerization: Can Control be Achieved?

2007 ◽  
Vol 60 (10) ◽  
pp. 788 ◽  
Author(s):  
Markus Busch ◽  
Marion Roth ◽  
Martina H. Stenzel ◽  
Thomas P. Davis ◽  
Christopher Barner-Kowollik
Keyword(s):  
Molecular Weight ◽  
High Pressure ◽  
High Temperature ◽  
Degree Of Polymerization ◽  
Molecular Weight Distributions ◽  
High Pressure High Temperature ◽  
Reversible Addition ◽  
Weight Distributions ◽  
Raft Agent ◽  
Initial Results

Simulations are employed to establish the feasibility of achieving controlled/living ethene polymerizations. Such simulations indicate that reversible addition–fragmentation chain transfer (RAFT) agents carrying a fluorine Z group may be suitable to establish control in high-pressure high-temperature ethene polymerizations. Based on these simulations, specific fluorine (F-RAFT) agents have been designed and tested. The initial results are promising and indicate that it may indeed be possible to achieve molecular weight distributions with a polydispersity being significantly lower than that observed in the conventional free radical process. In our initial trials presented here (using the F-RAFT agent isopropylfluorodithioformate), a correlation between the degree of polymerization and conversion can indeed be observed. Both the lowered polydispersity and the linear correlation between molecular weight and conversion indicate that control may in principle be possible.

Tertiary amine catalyzed photo-induced controlled radical polymerization of methacrylates

2015 ◽  
Vol 6 (30) ◽  
pp. 5362-5368 ◽  
Author(s):  
Qiang Fu ◽  
Thomas G. McKenzie ◽  
Shereen Tan ◽  
Eunhyung Nam ◽  
Greg G. Qiao
Keyword(s):  
Molecular Weight ◽  
Radical Polymerization ◽  
Uv Irradiation ◽  
Tertiary Amine ◽  
Controlled Radical Polymerization ◽  
Low Molecular Weight ◽  
Molecular Weight Distributions ◽  
Weight Distributions ◽  
End Group

A novel tertiary amine catalyst and trithiocarbonate synergistic photo-induced controlled radical polymerization of methacrylates has been realized under mild UV irradiation, yielding polymethacrylates with low molecular weight distributions and excellent end-group fidelity.

Molecular Weight Determinations Of Low Molecular Weight (LMW) Heparins By Ultracentrifugation And High Pressure Liquid Chromatography

1981 ◽  
Author(s):  
Grant Barlow ◽  
N Sugisaka ◽  
F J Petracek
Keyword(s):  
Molecular Weight ◽  
High Pressure ◽  
Liquid Chromatography ◽  
High Pressure Liquid Chromatography ◽  
Low Molecular Weight ◽  
Analytical Ultracentrifuge ◽  
Molecular Weights ◽  
Molecular Weight Distributions ◽  
Weight Distributions ◽  
Heparin Fractions

Molecular weights were independently determined on nitrous acid depolymerized LMW heparin fractions ranging from 2-15 daltons using the analytical ultracentrifuge and high pressure liquid chromatography (HPLC).Sedimentation-diffusion equilibria were obtained in the analytical ultracentrifuge using speeds ranging from 20,000 to 56,000 rpm. Near theta conditions were obtained using 0.5M NaCl as the solvent. Calculations of molecular weight distributions and, from those figures, weight average molecular weights were made using the method described by Scholte (N.Y. Acad Sci. 164, 156, 1969). The results show that weight average values as low as 2,000 daltons can be determined.Sedimentation-diffusion equilibria were obtained in the analytical ultracentrifuge using speeds ranging from 20,000 to 56,000 rpm. Near theta conditions were obtained using 0.5M NaCl as the solvent. Calculations of molecular weight distributions and, from those figures, weight average molecular weights were made using the method described by Scholte (N.Y. Acad Sci. 164, 156, 1969). The results show that weight average values as low as 2,000 daltons can be determined.The HPLC results were obtained using previously described methods (Fed Proc. 36, 89, 1977) and a new highly efficient gel column (TSK gels). Fractionated dextrans were used as reference standards.

Mechanical and Viscoelastic Characterization of Hyperbranched Polyisobutylenes

2002 ◽  
Vol 75 (5) ◽  
pp. 853-864 ◽  
Author(s):  
Judit E. Puskas ◽  
Christophe Paulo ◽  
Volker Altstädt
Keyword(s):  
Molecular Weight ◽  
Butyl Rubber ◽  
Structure Property ◽  
Carbocationic Polymerization ◽  
Molecular Weights ◽  
Structure Property Relationships ◽  
Molecular Weight Distributions ◽  
Weight Distributions ◽  
Living Carbocationic Polymerization

Abstract Structure-property relationships were investigated in hyperbranched polyisobutylenes, in comparison with commercial linear butyl rubber. The gel-free, soluble hyperbranched polyisobutylenes, synthesized by living carbocationic polymerization, had molecular weights, Mw≈400,000 to 1,000,000 g/mol, molecular weight distributions, MWD ≈1.2 to 2.6, and branching frequencies, BR ≈ 4 to 60. The mechanical and viscoelastic characterization of these polymers revealed interesting properties, including the characteristics of crosslinked rubbers.

scholarly journals Preparation and Characterization of Poly(2-vinylpyridine) with Narrow Molecular Weight Distributions

1986 ◽  
Vol 18 (4) ◽  
pp. 361-366 ◽  
Author(s):  
Yushu Matsushita ◽  
Kunio Shimizu ◽  
Yasushi Nakao ◽  
Haruhisa Choshi ◽  
Ichiro Noda ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Molecular Weight Distributions ◽  
Weight Distributions

Synthesis and Properties of Uniform Polyisoprene Networks. I. Synthesis and Characterization of α,ω-Dihydroxy-Polyisoprene

1976 ◽  
Vol 49 (2) ◽  
pp. 303-319 ◽  
Author(s):  
M. Morton ◽  
L. J. Fetters ◽  
J. Inomata ◽  
D. C. Rubio ◽  
R. N. Young
Keyword(s):  
Molecular Weight ◽  
Physical Properties ◽  
Soluble Fraction ◽  
Synthesis And Characterization ◽  
Molecular Weights ◽  
Molecular Weight Distributions ◽  
Weight Distributions ◽  
The Subject

Abstract The results of this study are the first to show that high-1,4 linear α,ω-dihydroxypolydienes can be synthesized with (a) predictable molecular weights, (b) narrow molecular weight distributions, and (c) high functionalities. Using the functionalized polyisoprenes prepared in this work, a series of networks was prepared with a purified triisocyanate as the chain linking agent. The soluble fraction in these networks ranged from 4.6 to 1.6 per cent. The characteristics and physical properties of these networks will be the subject of a forthcoming publication.

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