• Membrane Journal
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• v.23 no.2
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• pp.170-175
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• 2013

Poly (vinyl alcohol) (PVA) solution containing the glutaraldehyde (GA) as a crosslinking agent was coated onto the polyacrylonitrile (PAN) hollow fiber membrane as the supporter. Pervaporation experiments were carried out to characterize the prepared PVA/PAN composite membrane for water-isopropyl alcohol mixture. The flux and separation factor were measured at 30, 50, $90^{\circ}C$ for the feed mixture of aqueous 85 wt% IPA solution with varying the reaction temperature and composition of coating solutions. Typically the flux showed 1,870 $g/m^2{\cdot}hr$ at $90^{\circ}C$ feed mixture and the coating concentration of 3.5 wt% and the highest separation factor of 804 was obtained at $30^{\circ}C$ feed mixture and the coating concentration of 7 wt% as well.

• Membrane Journal
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• v.23 no.4
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• pp.283-289
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• 2013

Poly(vinyl alcohol) (PVA) coating solution containing glutaraldehyde (GA) and maleic anhydride (MA) as crosslinking agents was coated onto hydrolyzed poly acrylonitrile (PAN) hollow fiber membranes. The permselectivities of the resulting composite membranes prepared varying the reaction temperature and the concentration of the crosslinking agents were tested for 90 wt% ethanol aqueous mixtures by the pervaporation technique at $60^{\circ}C$. In general, the flux decreased while the selectivity increased for the increases of the reaction temperature and the crosslinking concentration. In case of GA as a crosslinking, the flux $165g/m^2hr$ and the separation factor 81 were obtained at GA 11 wt% and the reaction temperature $120^{\circ}C$. And for the case of MA, the flux $174g/m^2hr$ and the separation factor 73 were obtained at MA 11 wt% and the reaction temperature $120^{\circ}C$.

• Journal of Chest Surgery
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• v.46 no.1
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• pp.1-13
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• 2013

Background: Glutaraldehyde (GA) is a widely used cross-linking agent for improving mechanical properties and resistance to enzymatic degradation of collagenous tissue, but it has several drawbacks such as calcification and cytotoxicity. The aim of this study was to find the alternative effective cross-linking methods to GA. Materials and Methods: Bovine pericardium was processed with GA with ethanol+octanol and glycine detoxification, and polyethylene glycol (PG) space filler, dimethyl 3,3'-dithiobispropionimidate (DTBP), 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) treatment, and the physical fixation of ultraviolet irradiation were done. The biologic material properties of variously treated pericardial tissues were assessed by biochemical, mechanical and histological tests. Treated pericardial tissues were also implanted subcutaneously or intramuscularly into the rabbit for 10 weeks to assess the xenoreactive antibody response of immunoglobulin G and M, their anti-calcification effect. Results: The biochemical and mechanical properties of EDC fixed pericardial tissues were comparable to the GA fixed tissue. The cytotoxicity was lowest in space filler treated GA fixed group. In rabbit subcutaneous or intramuscular implantation models, decellularization, space filler, EDC treatment group showed significantly lower calcium content than GA only and DTBP treatment group (p<0.05, analysis of variance). The titer of anti $Gal{\alpha}1-3Gal{\beta}1$-4GlcNAc-R antibodies did not change in the postimplantation serial enzyme-linked immunosorbent assay. Hematoxylin and eosin and von Kossa staining showed that decellularization, space filler, EDC, and ultraviolet treatment had less inflammatory cell infiltration and calcium deposits. Conclusion: The decellularization process, PG filler, and EDC treatments are good alternative cross-linking methods compared to GA only fixation and primary amine of DTBP treatment for cardiovascular xenograft preservation in terms of the collagen cross-linking stability and in vivo anti-calcification effects.

• Journal of Chest Surgery
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• v.31 no.6
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• pp.560-566
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• 1998

Background: Bovine pericardial bioprosthesis treated with glutaraldehyde (GA) is one of the most popular prosthetic materials, but late calcific degeneration after implantation is a problem that remains unsolved. For the purpose of mitigating the calcific degeneration, we added MgCl2 into the 0.625% GA solution to compete with calcium for binding to the free aldehyde from GA and pretreated with the surfactants like sodium dodecyl sulfate (SDS) and Triton X-100 before GA fixation for preventing the phospholipid infiltration into the pericardial tissue, the first step of the calcific degeneration. Material and Method: 40 square-shaped pieces of bovine pericardia were fixed in 0.625% GA solution with 4g/L MgCl2 6H2O as a control group (group 1). 40 pieces pretreated with 1% SDS were also fixed in the same GA solution (group 2) and other 40 pieces pretreated with 1% Triton X-100 were prepared with the same method (group 3). After 1 month of fixation these were implanted into the belly of 40 Sprague-Dawley subdermally and extracted 1 month, 2 months, 3 months and 6 months after implantation. With atomic absorption spectrophotometry we measured the deposited calcium amount. Result: 1 month after implantation we could not find any differences between the three groups, but by the 2nd month calcium deposition was 0.921$\pm$0.121 mg/g in group 1, 0.481$\pm$0.037 mg/g in group 2 and 1.369$\pm$0.200 mg/g in group 3. By the 3rd month it was 0.786$\pm$0.080 mg/g in group 1, 0.584$\pm$0.054 mg/g in group 2 and 1.139$\pm$0.188 mg/g in group 3, and on the 6th month 1.623$\pm$0.601 mg/g in group 1,0.501$\pm$0.043 mg/g in group 2 and 1.625$\pm$0.382 mg/g in group 3, with statistical significance in group 2(p<0.05). Conclusion: Pretreatment with SDS showed meaningful calcium mitigation effects on subcutaneously implanted bovine pericardium in the rat models but the neutral type surfactant, Triton X-100, had no positive mitigation effect in this experiment.

• Journal of Chest Surgery
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• v.43 no.3
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• pp.235-245
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• 2010

Background: Our goal was to evaluate anti-calcification effects of decellularization and diverse fixing methods including preincubation of the bovine pericardium with ethanol. We also assessed changes in mechanical properties. Material and Method: Harvested bovine pericardium was decellularized with 0.25% sodim dodecysulfate and then treated with 5 methods of fixation: (1) 0.5% glutaraldehyde (GA) for 14 days, (2) 0.5% GA for 5 days, 2% GA for 2 days and 0.25% GA for 7 days, (3) 0.5% GA for 5 days, 2% GA for 2 days, 0.25% GA for 7 days, and then 70% ethanol for 2 days, (4) 0.5% GA for 5 days, a mixture of 2% GA and 70% ethanol for 2 days, and 0.25% GA for 7 days, (5) 0.5% GA for 5 days, a mixture of 2% GA, 65% ethanol, and 5% octanediol for 2 days and then 0.25% GA for 7 days. All treated bovine pericardia were tested for histological variables, lipid content, and mechanical properties including tensile strength and thermal stability. A total 10 kinds of differently treated bovine pericardia were implanted into rat subdermis and harvested 8 weeks later. Harvested pericardia were evaluated for calcium content. Result: No protein denaturation was observed microscopically after decellularization. There was a 32% mean decrease in tensile strength index after decellularization in the bovine pericardium group fixed. Octanediol preincubation attenuated the decrease in tensile strength and maintained thermal stability. TG and cholesterol were not affected by decellularization but were decreased by organic solvent. Calcium content was decreased after decellularization, and organic solvent preincubation decreased calcification in the non-decellularized bovine pericardium group. Conclusion: Decellularization and organic solvent preincubation have anti-calcification effects but decellularization may cause mechanical instability. A method of decellularization and fixation that does not cause damage to matrices will be needed for evaluation of the next step in using tissue-engineering for replacement of cardiac valves.

• Journal of Chest Surgery
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• v.43 no.6
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• pp.576-587
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• 2010

Background: Effective decellularization and fixation process is critical, in order to use xenogenic valves clinically. In the present study, we decellularized bovine pericardium using sodium dodecyl sulfate (SDS) and N-lauroyl sarcosinate, treated with $\alpha$-galactosidase, and then fixed in various manners, to find out the most effective tissue preservation & fixation procedure. Material and Method: Bovine pericardium was decellularized with SDS and N-lauroyl sarcosinate, and treated with $\alpha$-galactosidase. Both groups were fixed differently, by varying glutaraldehyde (GA) or EDC (1-ethyl-3-(3-dimethyl aminopropyl)-carbodiimide)/N-hydroxysuccinamide (NHS) treatment conditions. Thereafter, physical examination, tensile strength test, thermal stability test, cytotoxicity test, pronase test, pronase-ninhydrin test, purpald test, permeability test, compliance test, H&E staining, DNA quantification, and $\alpha$-galactose staining were carried out to each groups. Result: GA fixed groups showed better physical properties and thermal stability than EDC/NHS fixed groups, EDC/NHS-GA dual fixed groups showed better physical properties and thermal stability than EDC/NHS fixed groups, and showed better thermal stability than GA fixed groups. In pronase test and pronase-ninhydrin test, GA fixed groups and EDC/NHS-GA dual fixed groups showed stronger crosslinks than EDC/NHS groups. Permeability and compliance tended to increase in EDC/NHS-GA dual fixed groups, compared to GA fixed groups. But, EDC/NHS-GA dual fixed groups had stronger tensile strength and lower cytotoxicity than GA fixed groups. Conclusion: We have verified that EDC/NHS-GA dual fixation can make effective crosslinks and lower the toxicity of GA fixation. Henceforth, we will verify if EDC/NHS-GA dual fixation can lower calcifications & tissue failure in vivo experiment.

• Membrane Journal
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• v.33 no.6
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• pp.369-376
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• 2023

In this study, the alternative to the energy-intensive conventional vacuum distillation process, an eco-friendly and energy-efficient pervaporation separation was employed in 1,2 hexane diol/water (HDO/water) mixture. The crosslinked PVA-glutaraldehyde was coated inside the alumina hollow fiber membrane (Al-HF). In the HDO/IPA pervaporation separation, optimization of the membrane concerning PVA/GA ratio, curing temperature, and pervaporation operating condition were performed. In the long-term stability test, the sustainable pervaporation separation performance giving flux in the range of 1.90~2.16 kg/m²h, and water content in permeate was higher than 99.5% (separation factor = 68) was obtained from the PVA/GA (molar ratio = 0.08, curing temperature = 80℃) coated Al-HF membrane from HDO/water (25/75, w/w, %) mixture at 40℃. Therefore, this work provides potential and inspiration for PVA-based membranes to mitigate excessive energy requirements in HDO/water separation by pervaporation.

• Macromolecular Research
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• v.16 no.4
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• pp.373-378
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• 2008

A simple chemical fixation method for the fabrication of layer-by-layer (LbL) polyelectrolyte multilayer (PEM) has been developed to create a large area, highly uniform film for various applications. PEM of weak poly-electrolytes, i.e., polyallylamine hydrogen chloride (PAH) and poly(acrylic acid)(PAA), was assembled on polymer substrates such as poly(methyl methacrylate)(PMMA) and polycarbonate (PC). In the case of a weak polyelectrolyte, the fabricated thin film thickness of the polyelectrolyte multilayers was strongly dependent on the pH of the processing solution, which enabled the film thickness or optical properties to be controlled. On the other hand, the environmental stability for device application was poor. In this study, we utilized the chemical fixation method using glutaraldehyde (GA)-amine reaction in order to stabilize the polyelectrolyte multilayers. By simple treatment of GA on the PEM film, the inherent morphology was fixed and the adhesion and mechanical strength were improved. Both surface tension and FT-IR measurements supported the chemical cross-linking reaction. The surface property of the polyelectrolyte films was altered and converted from hydrophilic to hydrophobic by chemical modification. The possible application to antireflection coating on PMMA and PC was demonstrated.

• Journal of Chest Surgery
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• v.42 no.6
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• pp.685-695
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• 2009

Background: Calcification is the most frequent cause of clinical failure of bioprosthetic tissues that are fabricated from Glutaraldehyde (GA)-fixed porcine valve or bovine pericardium. We recently used a multi-factorial approach of employing different mechanisms to investigate how to reduce the calcification of bioprosthetic tissues. The purpose of the present study was to evaluate the synchronized synergism using ethanol, L-lysine and $NaBH_4$ in glutaraldehyde treated porcine pericardium from the standpoint of calcification and tissue elasticity. Material and Method: Porcine pericardium was fixed with 0.625% GA (commercial fixation). An interim step of ethanol (80%; 1 day at room temperature) or L-lysine (0.1 M; 2 days at $37^{\circ}C$) or $NaBH_4$ (0.1 M; 2 days at room temperature) was followed by completion of the GA fixation (2 days at $4^{\circ}C$ and 7 days at room temperature). The tensile strength and thickness of the samples were measured. The treated pericardiums were implanted subcutaneously into three-week old Sprague-Dawley rats for 8 weeks. The calcium content was assessed by atomic absorption spectroscopy and the histology of the samples. Result: The amount of calcium in the pericardium pretreated with ethanol (13.6${\pm}$10.0 ug/mg, p=0.008), L-lysine (15.3${\pm}$1.0 ug/mg, p=0.002) and both (16.1${\pm}$11.1 ug/mg, p=0.012) was significantly reduced compared with the control (51.2${\pm}$8.5 ug/mg). However, $NaBH_4$ pretreatment (65.7${\pm}$61.8 ug/mg, p=0.653) and combined pretreatment that including ethanol, L-lysine and $NaBH_4$ (92.9${\pm}$58.3 ug/mg, p=0.288) were not significantly different from the controls(51.2${\pm}$8.5 ug/mg). Both the combined pretreatment using ethanol and L-lysine (7.60${\pm}$1.55, p=0.76) and the combined pretreatment that included ethanol, L-lysine and $NaBH_4$ (7.47${\pm}$1.85, p=0.33) increased the tensile strength/thickness ratio compared with that of the controls (4.75${\pm}$1.88). Conclusion: The combined pretreatment using ethanol and L-lysine seemed to decrease the calcification of porcine pericardium fixed with glutaraldehyde, as compared to single pretreatment, and it increase the tissue elasticity, but to the degree that showed synchronized synergism. $NaBH_4$ pretreatment seemed to increase the calcification of porcine pericardium, irrespective of whether single or combined pretreatment was used.

• Membrane Journal
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• v.14 no.2
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• pp.166-172
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• 2004

As a preliminary study for esterification membrane reactor used to produce 2,2,2-trifluoroethylmetacrylate (TFEMA), Pervaporation behaviors with crosslinked Poly(vinyl alcohol) composite membranes were investigated for aqueous TFEA (2,2,2-trifluoroethanol) feed solutions. In this study, crosslinked PVA composite membranes were prepared by reacting PVA with glutaraldehyde (CA)/acid catalyst onto porous polyethersulfone (PES) supports. SEH images (scanning electron microscopy) showed the thicknesses of selective coating layer was about 2-3 ${\mu}{\textrm}{m}$. The swelling tests showed the dogree of crosslinking decreased as content of the crosslinking agent, GA, increased. Total permeation flux decreased while separation factor increased as the CA content increased. As operating temperature increased, total permeation flux remarkably increased in the range of 85-95 wt% TFEA aqueous solutions. Interestingly, however, separation factor decreased in 85-90 wt% with operating temperature, while that increased in 95 wt%. In case of 90 wt% TFEA concentration and operating temperature 8$0^{\circ}C$, the PVA composite membrane crosslinked with 0.1 mol GA per PVA repeating unit showed high permeation flux of 1.5 kg/$m^2$hr and separation factor of 320. These results confirmed the applicability of the PVA composite membranes for the esterification membrane reactor of TFEMA.