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PubMed1989

Effect of protein side chain amide group on the hydrogen-bond equilibrium in nucleobases studied by infrared and 13C-NMR spectroscopy.

Infrared spectra of 1:1 hydrogen-bonded complexes formed by derivatives of adenine and model molecules bearing the protein side chain amide group have been measured in chloroform solution. From the temperature dependence of hydrogen-bond formation, thermodynamic data on these complexes are determined. On the basis of these data, it is shown that the complexes consist of cyclic heterodimers, those that use the adenine N(1)H bond being favoured. Similarly infrared and 13C-NMR spectroscopy reveals that uracil-amide cyclic heterodimers formed through the uracil 4-carbonyl group are predominant. All of these results predict that Watson-Crick hydrogen bonds in adenine-uracil base-pairs may be opened to some extent, as proved in this work. The possible biological importance of these observations is also discussed.

Acetamides↗

PubMed2004

Scanning electron microscopic studies of Supramid Extra from the patients displaying recurrent ptosis after frontalis suspension.

PURPOSE: To investigate the morphologic changes in Supramid Extra suture harvested from patients displaying recurrent ptosis who had undergone a frontalis suspension for congenital ptosis. DESIGN: Observational case series. METHODS: Using scanning electron microscopy, we examined the morphologic changes in Supramid Extra (S. Jackson Inc, Alexandria, Virginia, USA) harvested from 20 consecutive patients (23 eyelids) with recurrent ptosis who had undergone frontalis suspension. Disintegration was graded as mild, moderate, or severe. RESULTS: Examination of unused Supramid showed the smooth surface of the sheath and round, well-demarcated polyfilaments on cross section. However, implanted Supramid showed different degrees of disintegration. The surface of the sheath had a rough texture with cracks and peeling. On cross section, an accumulation of debris among the polyfilaments and irregular architectures with decreased diameters of the polyfilaments were noted in some cases. On the surface of polyfilaments, different degrees of debris were noted in all cases. The degree of the changes was not exactly correlated with either the time of the recurrence or the duration of implantation. However, as the duration of implanted Supramid increased, greater changes on the surface of the sheath were noted. With implantation of less than 37 months, mild changes (44%) were predominant; between 37 and 48 months, moderate changes (60%) were noted, and with more than 48 months of implantation, severe changes (44%) were predominant. CONCLUSIONS: Supramid undergoes morphologic degradation by hydrolysis after implantation. This change might be considered one of the possible factors that facilitate the recurrence of ptosis.

Adolescent↗

PubMed2005

Cytotoxicity of thermosensitive polymers poly(N-isopropylacrylamide), poly(N-vinylcaprolactam) and amphiphilically modified poly(N-vinylcaprolactam).

Thermosensitive polymers poly(N-isopropylacrylamide) (PNIPAM), poly(N-vinylcaprolactam) (PVCL) and PVCL grafted with amphiphilic poly(ethylene oxide) (PEO) chains (PVCL-graft-C11EO42) were prepared and characterized and their putative cytotoxicity was evaluated. The cytotoxicity of these thermosensitive polymers and their monomers was investigated as a function of polymer concentration, incubation time and incubation temperature by using 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and lactate dehydrogenase (LDH) cytotoxicity tests in Caco-2 and Calu-3 cell cultures. Also, the influence of the chain end functionality on toxicity was examined. Viability (MTT) and cellular damage (LDH) of the cells were shown to be dependent on the surface properties of the polymers, hydrophilicity or hydrophobicity. Hydrophilic PVCL and PVCL-graft-C11EO42 were well tolerated at all polymer concentrations (0.1-10.0 mg/ml) after 3 h of incubation at room temperature and at physiological temperature (37 degrees C). The more hydrophobic PNIPAM induced more clear cellular cytotoxicity at 37 degrees C. The monomers N-isopropylacrylamide and vinylcaprolactam and PEO-macromonomer showed dramatically higher cytotoxicity values with respect to the corresponding polymers. Cell damage was directly dependent on concentration, temperature and incubation time.

Acrylic Resins↗

PubMed2005

Formation of bone-like apatite on organic polymers treated with a silane-coupling agent and a titania solution.

Polyethylene terephthalate (PET), ethylene-vinyl alcohol copolymer (EVOH) and Nylon 6 in plate form were treated with silane-coupling agents, a titanium alkoxide-alcohol solution and a hot HCl solution to form a thin crystalline titanium oxide layer. When placed in a simulated body fluid with ion concentrations nearly equal to those of the human blood plasma, nanosized bone-like apatite formed uniformly on the surfaces of these treated polymers: within 2 days for PET and Nylon 6, and 7 days for EVOH. This indicates that such titania-modified polymers might form bone-like apatite in the living body, and bond to living bone through this apatite layer. Three-dimensional fabrics of these polymer fibers, with open spaces in various sizes, are expected to be useful as bone substitutes, as they will be integrated with the natural bone.

Apatites↗

PubMed2006

Phase-transition and aggregation characteristics of a thermoresponsive dextran derivative in aqueous solutions.

Grafting of poly(N-vinylcaprolactam) side chains onto a hydrophilic dextran backbone was found to provide the dextran with new, thermoresponsive properties in aqueous solutions. Depending on its solution concentration, the resulting dextran derivative could exhibit a temperature-induced phase-transition and critical transition temperature (T(c)). Different anions and cations of added salts, including five potassium salts and five alkali-metal chlorides, were observed to influence the T(c) value of its aqueous solution. Except for potassium iodide, all added salts were found to lower the T(c) value. The addition of the surfactant, cationic cetyltrimethylammonium bromide or anionic sodium dodecyl sulfate, resulted in an increase of the T(c) value. With the help of the Coomassie Brilliant Blue dye as a polarity probe, the formation of hydrophobic aggregates above the T(c) was revealed for this new dextran derivative in aqueous solution.

Caprolactam↗

PubMed2006

Films coated with molecular imprinted polymers for the selective stir bar sorption extraction of monocrotophos.

The flexibility and simplicity of stir bar sorption extraction (SBSE) have been combined with the selectivity of molecularly imprinted polymers (MIP). Stir bars were coated reproducible with a 180 microm film formed from a formic acid solution of nylon-6 polymer either nonimprinted or imprinted with monocrotophos. Time sorption profiles were measured for the extraction of monocrotophos from dichloromethane at the concentration of 10-200 micromol/L levels with both types of films in order to compare extraction characteristics. The results indicated that the MIP coated layer showed remarkable high affinity toward monocrotophos and equilibrium adsorption was attained rapidly (60 min) in contrast to free standing molecularly imprinted polymer in which equilibrium adsorption was normally attained after several hours. The stir bars coated with MIP films were capable of extracting four structural analogues of monocrotophos from dichloromethane solution, which suggests that both the amino group and PO part of these molecules is responsible for interaction with the imprinted polymer. Evidence was also presented by FT-IR analysis that the amide-hydrogen-bonding interaction between the MIP-coated films and monocrotophos was originated for monocrotophos recognition. To achieve selective extraction of monocrotophos from sample, stir bars coated with MIP films were washed with 10% (v/v) acetic acid/methanol and methanol. Clean extracts and yields of 95% were obtained, demonstrating the suitability of stir bar coated with MIP films for the analysis of environmental and biological samples. Compared with traditional MIP and SBSE, the MIP-coated film showed not only the high selectivity but also the rapid equilibrium adsorption.

Caprolactam↗

PubMed2026

Degradation of a graphene-reinforced polyamide by fungi: When culture conditions matter.

The large-scale production, marketing and disposal of polymer-based graphene products can lead to the dispersal of graphene-enriched plastic particles into terrestrial ecosystems, where they might accumulate if not degraded by organisms. The objective of this work is to test the degradability and compatibility of one polyamide-6 polymer reinforced with reduced graphene-oxide (PA6-rGO) and its base constituents (polyamide-6, PA6; reduced graphene oxide, rGO) using mono- and co-cultures of two lignin-degrading fungi (Bjerkandera adusta and Morchella esculenta) grown under different nutrient conditions. Fungal (co-)cultures were exposed to pure rGO or abraded powders of PA6 and PA6-rGO in two different liquid media, and monitored over time for biomass growth, H2O2 production, and activity of two lignolytic enzymes (i.e., Laccase, Lac, and Lignin peroxidase, LiP). The changes in polyamide structure were evaluated by proton nuclear magnetic resonance and mass spectrometry, and changes in rGO were evaluated by Raman spectroscopy. The materials had no effect on fungal growth. PA6 increased Lac secretion only in low nutrient medium, while PA6-rGO slightly suppressed LiP activity. Only M. esculenta promoted polyamides oxidation when cultured in a low nutrient medium, as evidenced by a change in mass distribution values (m/z: 400-420) and the appearance of a new resonance peak (at 5.37 ppm). Lignolytic exudates in co-cultures low in nutrients caused a greater change in rGO, as shown by the increase in the ID/IG ratio. The degradation of rGO, PA6 and PA6-rGO depended on culture conditions.

Graphite↗

PubMed2006

Experimental validation of a T2rho transverse relaxation model using LASER and CPMG acquisitions.

The transverse relaxation rate (R2=1/T2) of many biological tissues are altered by endogenous magnetized particles (i.e., ferritin, deoxyhemoglobin), and may be sensitive to the pathological progression of neurodegenerative disorders associated with altered brain-iron stores. R2 measurements using Carr-Purcell-Meiboom-Gill (CPMG) acquisitions are sensitive to the refocusing pulse interval (2taucp), and have been modeled as a chemical exchange (CE) process, while R2 measurements using a localization by adiabatic selective refocusing (LASER) sequence have an additional relaxation rate contribution that has been modeled as a R2rho process. However, no direct comparison of the R2 measured using these two sequences has been described for a controlled phantom model of magnetized particles. The three main objectives of this study were: (1) to compare the accuracy of R2 relaxation rate predictions from the CE model with experimental data acquired using a conventional CPMG sequence, (2) to compare R2 estimates obtained using LASER and CPMG acquisitions, and (3) to determine whether the CE model, modified to account for R2rho relaxation, adequately describes the R2 measured by LASER for a full range of taucp values. In all cases, our analysis was confined to spherical magnetic particles that satisfied the weak field regime. Three phantoms were produced that contained spherical magnetic particles (10 microm diameter polyamide powders) suspended in Gd-DTPA (1.0, 1.5, and 2.0 mmol/L) doped gel. Mono-exponential R2 measurements were made at 4T as a function of refocusing pulse interval. CPMG measurements of R2 agreed with CE model predictions while significant differences in R2 estimates were observed between LASER and CPMG measurements for short taucp acquisitions. The discrepancy between R2 estimates is shown to be attributable to contrast enhancement in LASER due to T2rho relaxation.

Calibration↗

PubMed2005

Removal of organic contaminants by RO and NF membranes.

Rejection characteristics of organic and inorganic compounds were examined for six reverse osmosis (RO) membranes and two nanofiltration (NF) membranes that are commercially available. A batch stirred-cell was employed to determine the membrane flux and the solute rejection for solutions at various concentrations and different pH conditions. The results show that for ionic solutes the degree of separation is influenced mainly by electrostatic exclusion, while for organic solutes the removal depends mainly upon the solute radius and molecular structure. In order to provide a better understanding of rejection mechanisms for the RO and NF membranes, the ratio of solute radius (r(i,s)) to effective membrane pore radius (r(p)) was employed to compare rejections. An empirical relation for the dependence of the rejection of organic compounds on the ratio r(i,s)/r(p) is presented. The rejection for organic compounds is over 75% when r(i,s)/r(p) is greater than 0.8. In addition, the rejection of organic compounds is examined using the extended Nernst-Planck equation coupled with a steric hindrance model. The transport of organic solutes is controlled mainly by diffusion for the compounds that have a high r(i,s)/r(p) ratio, while convection is dominant for compounds that have a small r(i,s)/r(p) ratio.

2-Propanol↗

PubMed2005

Thermal pyrolysis of fresh and waste fishing nets.

Kinetic tests on the pyrolysis of nylon-6 taken from fresh (new) fishing nets and waste fishing nets were conducted using thermogravimetric analysis at heating rates of 0.5, 1.0 and 2.0 degrees C/min. The main region of decomposition of both materials was between 340 and 440 degrees C at each heating rate. The region of decomposition for the nylon-6 from the waste fishing nets was slightly lower than that of the fresh fishing nets. The result shows that the value of activation energies increased from 128 to 433 kJ mol(-1) as the conversion of the pyrolysis reaction increased from 5% to 95%. Nylon-6 from the fresh fishing nets was pyrolyzed in a micro-scale tubing bomb reactor for 60, 80 and 100 min at 440 degrees C. The yield of pyrolyzed gases increased from 3.94 to 5.50 wt% with reaction time. The selectivity to specific hydrocarbons was not detected from the pyrolyzed oil and the carbon number distribution of the pyrolyzed oil was random.

Animals↗

PubMed2000

Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method. I. Injection procedure and column stability.

We report a method for reliable routine polymer sample introduction with minimal bias, a separation method of the first six linear and cyclic oligomers by liquid chromatography, quantification using group equivalents and long term method performance. Injecting a polymer sample in a mobile phase containing an aqueous non-solvent often results in blocked systems as the polymer precipitates in the connecting capillaries. In this first part we focus on a new injection technique, in which the dissolved polyamide is placed between two zones of formic acid, preventing the polymer to precipitate before it reaches the column. Development of this sandwich injection method makes direct injection of the polymer into an aqueous acetonitrile gradient feasible. The oligomeric polyamide recovery of this technique, extraction, dissolution/precipitation and direct injection on a hexafluoro-isopropanol (HFIP) gradient were compared. With the sandwich injection method the polymer remains on the column, slowly changing the stationary phase. The influence of this on resolution and retention was studied. Column stability allows sixty injections before cleaning or replacing the column is necessary.

Acetonitriles↗

PubMed2000

Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method. II. Methods of detection and quantification and overall long-term performance.

By separating the first six linear and cyclic oligomers of polyamide-6 on a reversed-phase high-performance liquid chromatographic system after sandwich injection, quantitative determination of these oligomers becomes feasible. Low-wavelength UV detection of the different oligomers and selective post-column reaction detection of the linear oligomers with o-phthalic dicarboxaldehyde (OPA) and 3-mercaptopropionic acid (3-MPA) are discussed. A general methodology for quantification of oligomers in polymers was developed. It is demonstrated that the empirically determined group-equivalent absorption coefficients and quench factors are a convenient way of quantifying linear and cyclic oligomers of nylon-6. The overall long-term performance of the method was studied by monitoring a reference sample and the calibration factors of the linear and cyclic oligomers.

Caprolactam↗

PubMed2001

Separation and quantification of the linear and cyclic structures of polyamide-6 at the critical point of adsorption.

The linear and cyclic structures of polyamide-6 were separated by liquid chromatography at critical conditions (LCCC) and identified with different mass spectrometric (MS) techniques and quantitated by LCCC with evaporative light-scattering detection (ELSD). Electrospray ionization MS was not suitable to identify the higher cyclic structures. For this purpose, matrix-assisted laser desorption ionization time-of-flight MS performed better and cyclic and linear structures were oligomerically resolved and separately identified in the mass spectrometer. The highest cyclic structure present and detected was the cyclic pentacontamer. It could be demonstrated that cyclic and linear oligomers follow different ionization and fragmentation routes/patterns. Quantification with ELSD of the components separated by LCCC using a universal calibration curve or an iterative procedure was developed. An area correction to account for different peak widths of coeluting components improves precision and accuracy of the calibration curve and improves quantitation accuracy for the samples analyzed. With these corrected values, no molecular mass dependency was observed for the cyclic and linear structures. Under critical conditions, the linear and cyclic structures of polyamide-6 were separated, identified and quantified.

Adsorption↗

PubMed2001

Headspace solid-phase microextraction--a tool for new insights into the long-term thermo-oxidation mechanism of polyamide 6.6.

Low-molecular-mass products formed during thermo-oxidation of polyamide 6.6 at 100 degrees C were extracted by headspace solid-phase microextraction and identified by GC-MS. A total of 18 degradation products of polyamide 6.6 were identified. In addition some low-molecular-mass products originating from the lubricants were detected. The identified degradation products were categorized into four groups where compounds within each group contain the same structural feature. In groups A, B and C several new thermo-oxidation products of polyamide 6.6 were identified including cyclic imides, pyridines and structural fragments from the original polyamide chain. 1-Pentyl-2,5-pyrrolidinedione (pentylsuccinimide) showed the largest increase in abundance during oxidation. The cyclopentanones in group D were already present in the un-aged material. Their amounts decreased during ageing and they are thus not formed during thermo-oxidation of polyamide 6.6 at 100 degrees C. The identified thermo-oxidation products can be formed as a result of extensive oxidation of the hexamethylenediamine unit in the polyamide backbone. The degradation products pattern shows that the long-term thermo-oxidative degradation, just like thermal degradation and photo-oxidation of polyamide 6.6, starts at the N-vicinal methylene groups.

Caprolactam↗

PubMed2002

Analysis of linear and cyclic oligomers in polyamide-6 without sample preparation by liquid chromatography using the sandwich injection method. III. Separation mechanism and gradient optimization.

The first six linear and cyclic oligomers of polyamide-6 can be quantitatively determined in the polymer using HPLC with the sandwich injection method and an aqueous acetonitrile gradient. In this final part of the triptych concerning the determination of the oligomers in polyamide-6, the irregular elution behavior of the cyclic monomer compared to the cyclic oligomers was investigated. We also optimized the separation of the involved polyamide oligomers, with respect to gradient steepness, stationary phase, column temperature and mobile phase pH. The irregular elution behavior of the cyclic monomer could be caused by its relatively large exposed/accessible hydrophobic surface, which permits relatively easy penetration into the hydrophobic stationary phase giving extra retention. The dipole moment of the different oligomers was used as a measure for this exposed/accessible hydrophobic area to correlate the retention factors using quantitative structure-retention relationships. We also studied the retention behavior of the polyamide, which is injected each run directly onto the column and modifies the stationary phase. Using a 250-microl post gradient injection zone of formic acid on a 250x3 mm Zorbax SB-C18 column, the polyamide could be effectively removed from the stationary phase after each separation. The linear solvent strength (LSS) model was used to optimize the separation of the first six linear and cyclic oligomers. As the LSS model assumes a linear correlation between the modifier concentration and the logarithm of the retention factor and the cyclic monomer and dimer show extreme curvation of this relation in the eluting region, we investigated different models to predict gradient elution from isocratic data. A direct translation of the isocratic data to gradient retention times did not yield adequate retention times using the LSS model. It was found that the LSS model worked acceptably if gradient retention times were used as input data. Even for fast non-linearly eluting components, an average error of 0.4 resolution units of 4sigma was obtained. Using the LSS model in combination with different column temperatures and mobile phase pH values, a separation of the first six linear and cyclic oligomers was accomplished.

Caprolactam↗

PubMed2002

Endgroup-based separation and quantitation of polyamide-6,6 by means of critical chromatography.

Polyamide-6,6 is a polycondensation product from the two monomers adipic acid and 1,6-hexamethylenediamine. Depending on the reacted amount of these monomers, different ratios of amine and carboxylic acid endgroups can be formed. Besides linear chains, cyclic polyamides will also be formed. Using critical chromatography, polyamide-6,6 can be separated independently of molar mass. Retention is based solely on endgroup functionality. It is demonstrated that high-molecular-mass polyamide-6,6 (Mw approximately 20,000-30,000) can be separated using this approach. The separation was optimized by using different parameters, such as percentage modifier, temperature and pressure. The concentration of phosphoric acid was used for selective retention of the different endgroup functionalities. Using this property, a new method called critical gradient chromatography was performed where the mobile phase changes from a weak to a strong solvent with respect to the endgroup functionality, while retaining the critical conditions of the backbone unit. Quantification using UV detection is discussed.

Caprolactam↗

PubMed2000

Analysis of higher polyamide-6 oligomers on a silica-based reversed-phase column with a gradient of formic acid as compared with hexafluoroisopropanol.

The analysis of polyamide-6 oligomers and polymer is usually performed with expensive fluorinated alcohols like 2,2,2-trifluoroethanol (TFE) or 1,1,1,3,3,3-hexafluoroisopropanol (HFIP). Formic acid is well known as a mobile phase additive to adjust pH in reversed-phase high-performance liquid chromatography. However, formic acid is seldom used as a modifier to perform gradient elution chromatography on octadecyl-modified silica-based columns. Here we demonstrate the determination of cyclic and linear polyamide-6 oligomers using formic acid as a modifier on an octadecyl-modified silica-based column. This column was shown to be stable for more than 5000 column volumes, even when a mobile phase of 65-95% formic acid in water at a flow of 1 ml/min is applied. With formic acid under the conditions used (65-95% formic acid in water) the oligomers are retained on the column, while the polymer does not precipitate. In comparison, during adsorption and separation with a HFIP gradient, precipitation of the polymer occurs. The implications of the different separation mechanisms, i.e., adsorption vs. precipitation chromatography are discussed. Loadability is shown to be much better with the formic acid system. However, with formic acid as a modifier UV detection below 250 nm is not feasible. The less sensitive evaporative light scattering detector is used to detect the polyamide oligomers in the formic acid phase. In addition it is shown that capillary zone electrophoresis (CZE) with UV-absorbance detection using HFIP is an attractive combination as HFIP is UV-transparent and CZE allows low modifier consumption.

Caprolactam↗

PubMedDate not supplied

Technical considerations in knot construction. Part I. Continuous percutaneous and dermal suture closure.

The purpose of this investigation was to determine the security of the square knot tied with one looped end and one free end versus the security of the square knot tied with two free ends. Size 4/0 and size 6/0 monofilament nylon, polypropylene, and Biosyn sutures were selected for this evaluation. The mechanical performance of these sutures was judged according to knot breakage force and number of throws required to attain security. Knots with one looped end and one free end require more throws to ensure knot security than do knots constructed from two single suture strands of comparable sizes and types of sutures.

Caprolactam↗