scholarly journals Enzymatic Synthesis of Poly(alkylene succinate)s: Influence of Reaction Conditions

Processes ◽  
2021 ◽  
Vol 9 (3) ◽  
pp. 411
Author(s):  
Doris Pospiech ◽  
Renata Choińska ◽  
Daniel Flugrat ◽  
Karin Sahre ◽  
Dieter Jehnichen ◽  
...  
Keyword(s):  
Molar Mass ◽  
Toxic Metal ◽  
Dicarboxylic Acids ◽  
Size Exclusion ◽  
Butylene Succinate ◽  
Aliphatic Polyesters ◽  
Synthesis Conditions ◽  
Melt Polycondensation ◽  
Exclusion Chromatography ◽  
Immobilized Calb

Application of lipases (preferentially Candida antarctica Lipase B, CALB) for melt polycondensation of aliphatic polyesters by transesterification of activated dicarboxylic acids with diols allows to displace toxic metal and metal oxide catalysts. Immobilization of the enzyme enhances the activity and the temperature range of use. The possibility to use enzyme-catalyzed polycondensation in melt is studied and compared to results of polycondensations in solution. The experiments show that CALB successfully catalyzes polycondensation of both, divinyladipate and dimethylsuccinate, respectively, with 1,4-butanediol. NMR spectroscopy, relative molar masses obtained by size exclusion chromatography, MALDI-TOF MS and wide-angle X-ray scattering are employed to compare the influence of synthesis conditions for poly(butylene adipate) (PBA) and poly(butylene succinate) (PBS). It is shown that the enzymatic activity of immobilized CALB deviates and influences the molar mass. CALB-catalyzed polycondensation of PBA in solution for 24 h at 70 °C achieves molar masses of up to Mw~60,000 g/mol, higher than reported previously and comparable to conventional PBA, while melt polycondensation resulted in a moderate decrease of molar mass to Mw~31,000. Enzymatically catalyzed melt polycondensation of PBS yields Mw~23,400 g/mol vs. Mw~40,000 g/mol with titanium(IV)n-butoxide. Melt polycondensation with enzyme catalysis allows to reduce the reaction time from days to 3-4 h.

scholarly journals Comprehensive characterization and quantification of adeno associated vectors by size exclusion chromatography and multi angle light scattering

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Nicole L. McIntosh ◽  
Geoffrey Y. Berguig ◽  
Omair A. Karim ◽  
Christa L. Cortesio ◽  
Rolando De Angelis ◽  
...  
Keyword(s):  
Light Scattering ◽  
Size Exclusion Chromatography ◽  
Molar Mass ◽  
Size Exclusion ◽  
Minimal Sample ◽  
Accuracy And Precision ◽  
Vector Genome ◽  
Exclusion Chromatography ◽  
Novel Applications

AbstractAdeno associated virus (AAV) capsids are a leading modality for in vivo gene delivery. Complete and precise characterization of capsid particles, including capsid and vector genome concentration, is necessary to safely and efficaciously dose patients. Size exclusion chromatography (SEC) coupled to multiangle light scattering (MALS) offers a straightforward approach to comprehensively characterize AAV capsids. The current study demonstrates that this method provides detailed AAV characterization information, including but not limited to aggregation profile, size-distribution, capsid content, capsid molar mass, encapsidated DNA molar mass, and total capsid and vector genome titer. Currently, multiple techniques are required to generate this information, with varying accuracy and precision. In the current study, a new series of equations for SEC-MALS are used in tandem with intrinsic properties of the capsids and encapsidated DNA to quantify multiple physical AAV attributes in one 20-min run with minimal sample manipulation, high accuracy, and high precision. These novel applications designate this well-established method as a powerful tool for product development and process analytics in future gene therapy programs.

scholarly journals Molar mass characterization of hydrophilic copolymers, 2 Size exclusion chromatography of cationic (meth)acrylate copolymers

e-Polymers ◽  
2005 ◽  
Vol 5 (1) ◽  
Author(s):  
Martina Adler ◽  
Harald Pasch ◽  
Christian Meier ◽  
Raimund Senger ◽  
Hans-Günter Koban ◽  
...  
Keyword(s):  
Stationary Phase ◽  
Size Exclusion Chromatography ◽  
Molar Mass ◽  
Extended Period ◽  
Size Exclusion ◽  
Viscosity Data ◽  
Exclusion Chromatography ◽  
Reproducible Method ◽  
Novel Method ◽  
Sec System

AbstractA robust and reproducible method for the molar mass analysis of cationic copolymers based on dimethylaminoethyl methacrylate or trimethylammonioethyl methacrylate and different (meth)acrylates has been developed. Size exclusion chromatography (SEC) using a novel polyester-based packing as the stationary phase and dimethylacetamide (DMAC) as the mobile phase yields highly accurate results for copolymers with an amino comonomer content up to 50 wt.-%. To suppress the different polar and ionic interactions between sample molecules, stationary phase and eluent, DMAC was modified with LiBr and tris(hydroxymethylamino) methane (TRIS). Calibrating the SEC system with poly(methyl methacrylate) of narrow polydispersity, molar masses were obtained that are in good agreement with viscosity data. Reproducibility and robustness of the novel method were proven by running samples for an extended period of two weeks.

Consecutive determination of softwood kraft lignin structure and molar mass from NMR measurements

Holzforschung ◽  
2017 ◽  
Vol 71 (7-8) ◽  
pp. 563-570 ◽  
Author(s):  
Jerk Rönnols ◽  
Anna Jacobs ◽  
Fredrik Aldaeus
Keyword(s):  
Molar Mass ◽  
Industrial Applications ◽  
Size Exclusion ◽  
Ionization Time ◽  
Flight Mass Spectrometry ◽  
Exclusion Chromatography ◽  
Pfg Nmr ◽  
Softwood Kraft Lignin ◽  
Good Agreement

Abstract The general molecular properties and in particular, the molar mass of lignin are of central importance for industrial applications, as these data govern important thermal and mechanical characteristics. The focus of the present paper is pulsed field gradient-nuclear magnetic resonance (PFG-NMR), which is suitable for determination of lignins’ weight-average molar mass, based on diffusion constants. The method is calibrated by lignin fractions characterized by matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS). It could be demonstrated on a set of softwood kraft lignins that the PFG-NMR approach gives results in very good agreement with those obtained using conventional size exclusion chromatography (SEC).

Ring-Opening Polymerization of L-lactide Initiated by Samarium(III) Acetate

2019 ◽  
Vol 3 (2) ◽  
pp. 112-119
Author(s):  
Jesús Miguel Contreras Ramírez ◽  
Dimas Medina ◽  
Francisco López-Carrasquero ◽  
Ricardo Rafael Contreras
Keyword(s):  
1H Nmr ◽  
Ring Opening ◽  
Alkali Metals ◽  
Molar Mass ◽  
Ring Opening Polymerization ◽  
Solvent Free ◽  
Size Exclusion ◽  
Polymerization Process ◽  
Molar Ratio ◽  
Aliphatic Polyesters

Background: The synthesis of the aliphatic polyesters obtained by the ring opening polymerization has been achieved using as initiators a large amount of organometallic compounds derivative from: Alkali metals, alkaline earth metals, transition metals and lanthanide metals. Of all these compounds, the lanthanide derivatives have acquired great importance in the synthesis of aliphatic polyesters, since these show a greater catalytic activity and also can provide polymer with characteristics that will be very useful in the design of biomaterials. Objective: It was proposed the synthesis of poly(L-lactida) (PL-LA) through a ring opening polymerization process of L-lactide initiated with samarium(III) acetate (Sm(OAc)3) under solvent-free melt conditions. The influence of different parameters of reaction, such as temperature, time, molar ratio monomer to initiator, on typical variables of polymers, e.g., conversion, dispersity, and molar mass, were analyzed. Methods: All polymerizations were carried out under solvent-free melt conditions in ampoules-like flasks, equipped with a magnetic stirrer. The obtained polyesters were characterized by size exclusion chromatography (SEC) and 1H-NMR. Results: The Sm(OAc)3 induces the polymerization of L-LA at high conversion, and produce polyesters with number-average molecular weights of 1.00 x 103 to 30.00 x 103 Dalton. The 1H-NMR analysis indicates a typical polymerization mechanism of coordination-insertion, with a breakdown of the acyl-oxygen bond of the L-LA. Conclusion: Sm(OAc)3 was an effective initiator for the ring-opening polymerization of L-LA. SEC chromatography showed that, at high temperatures and prolonged reaction times, the molar mass of the polyester decreases, which is associated with the transesterification collateral reactions that occur during the polymerization process.

Influence of molecular structure on the rheological properties and foamability of long chain branched polypropylene by “one-pot” reactive extrusion

2020 ◽  
pp. 0021955X2094310
Author(s):  
Yan Li ◽  
Zhen Yao ◽  
Shaolong Qiu ◽  
Changchun Zeng ◽  
Kun Cao
Keyword(s):  
Coupling Reaction ◽  
Reactive Extrusion ◽  
Expansion Ratio ◽  
Size Exclusion ◽  
One Pot ◽  
Synthesis Conditions ◽  
Twin Screw ◽  
Exclusion Chromatography ◽  
In Series ◽  
Long Chain

In this work, reactive twin screw extrusion was conducted to synthesize long chain branched polypropylenes (LCB-PPs) in a “one-pot” process in which dicumyl peroxide (DCP) initiated maleic anhydride (MAH) grafting onto the linear PP, and the concomitant coupling reaction between ethylene diamine (EDA) and MAH grafted polypropylene (PP-g-MAH) proceeded in series. Fourier transfer infrared spectroscopy (FTIR) on the prepared materials confirmed the occurrence of both reactions. A series of LCB-PPs were prepared using different amounts of EDA, MAH and DCP to study their effects and determine the optimal synthesis conditions. The prepared materials were characterized by size exclusion chromatography (SEC) and rheological analysis to ascertain the polymer microstructure. The foamability of the LCB-PPs by supercritical carbon dioxide (scCO2) foaming and foam morphology were investigated. The LCB-PPs were found to have vastly improved foamability and cellular morphology. Under optimal conditions, a foam expansion ratio of over 20 was achieved.

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