Advantageous use of SFC for separation of crude therapeutic peptides and peptide libraries.

A simple SFC/MS (Supercritical Fluid Chromatography/Mass Spectrometry) method set was developed to effectively screen separations of various crude synthetic peptide products of pharmaceutical interest. Additives to the modifier methanol which were successful for these separations were found to include TFA (trifluoroacetic acid) and ammonia mixed with TFA, each at 0.1 % (v/v) composition in methanol. A final screening column set consisted of 2-ethylpyride (2-EP), 4-ethylpyridine (4-EP) and cross-linked diol (Luna™ HILIC) stationary phases. Small, linear and macrocyclic peptides with fewer than ten residues could all be eluted with good performance under at least one of the method conditions comprising the final screening protocol. For larger peptides either the 4-EP and HILIC columns with the above additives provided a good initial screening method set without 2-EP. The gradient was slightly longer and shifted to higher polarity relative to the gradients for smaller peptides. This method was often successful to elute large, hydrophilic peptides up to a 41-mer with acceptable peak profiles although the largest peptides with most ionizable residues were most challenging. For these peptides generally HILIC column performance was better with TFA + ammonia in the modifier than with TFA, while 4-EP performance was usually improved with TFA relative to TFA + ammonia.

The mixture of liquid foam soap, ethanol and citric acid as a new fixative-preservative solution in veterinary anatomy.

The present study investigates the efficiency of liquid foam soap, ethanol, citric acid and benzalkonium chloride as a fixative-preservative solution (a soap-and ethanol-based fixing solution, or SEFS). In this study, ethanol serves as the fixative and preservative, liquid foam soap as the modifying agent, citric acid as the antioxidant and benzalkonium chloride as the disinfectant. The goat cadavers perfused with SEFS (n=8) were evaluated over a period of one year with respect to hardness, colour and odour using objective methods. Colour and hardness were compared between one fresh cadaver and the SEFS-embalmed cadavers. Histological and microbiological examinations were also performed in tissue samples. Additionally, the cadavers were subjectively evaluated after dissection and palpation. The SEFS provided the effectiveness expected over a 1-year embalming period for the animal cadavers. No bacteria or fungi were isolated except for some non-pathogenic Bacillus species. Visible mould was not present on either cadavers or in the surrounding environment. The cadavers maintained an appearance close to their original anatomical appearance, with muscles having good hardness and elasticity for dissection.

Low-temperature dynamic nuclear polarization of gases in Frozen mixtures.

PURPOSE: To present a new cryogenic technique for preparing gaseous compounds in solid mixtures for polarization using dynamic nuclear polarization (DNP). METHODS: (129) Xe and (15) N2 O samples were prepared using the presented method. Samples were hyperpolarized at 1.42K at 5 Tesla. (129) Xe was polarized at 1.65K and 1.42K to compare enhancement. Polarization levels for both samples and T1 relaxation times for the (129) Xe sample were measured. Sample pulverization for the (129) Xe and controlled annealing for both samples were introduced as additional steps in sample preparation. RESULTS: Enhancement increased by 15% due to a temperature drop from 1.65K to 1.42K for the (129) Xe sample. A polarization level of 20 ± 3% for the (129) Xe sample was achieved, a two-fold increase from 10 ± 1% after pulverization of the sample at 1.42K. T1 of the (129) Xe sample was increased by more than three-fold by means of annealing. In the case of (15) N2 O, annealing led to a ∼two-fold increase in the signal level after DNP. CONCLUSION: The presented technique for producing and manipulating solid gas/glassing agent/radical mixtures for DNP led to high polarization levels in (129) Xe and (15) N2 O samples. These methods show potential for polarizing other gases using DNP technology. Magn Reson Med 76:1007-1014, 2016. © 2015 Wiley Periodicals, Inc.

Synthesis and characterization of carbon cryogel microspheres from lignin-furfural mixtures for biodiesel production.

The aim of this work was to study the potential of biofuel and biomass processing industry side-products as acid catalyst. The synthesis of carbon cryogel from lignin-furfural mixture, prepared via sol-gel polycondensation at 90°C for 0.5h, has been investigated for biodiesel production. The effect of lignin to furfural (L/F) ratios, lignin to water (L/W) ratios and acid concentration on carbon cryogel synthesis was studied. The carbon cryogels were characterized and tested for oleic acid conversion. The thermally stable amorphous spherical carbon cryogel has a large total surface area with high acidity. Experimental results revealed the optimum FAME yield and oleic acid conversion of 91.3wt.% and 98.1wt.%, respectively were attained at 65°C for 5h with 5wt.% catalyst loading and 20:1 methanol to oleic acid molar ratio. Therefore, carbon cryogel is highly potential for heterogeneous esterification of free fatty acid to biodiesel.

Tuning the degradation rate of calcium phosphate cements by incorporating mixtures of polylactic-co-glycolic acid microspheres and glucono-delta-lactone microparticles.

Calcium phosphate cements (CPCs) are frequently used as synthetic bone graft materials in view of their excellent osteocompatibility and clinical handling behavior. Hydroxyapatite-forming CPCs, however, degrade at very low rates, thereby limiting complete bone regeneration. The current study has investigated whether degradation of apatite-forming cements can be tuned by incorporating acid-producing slow-resorbing poly(D,L-lactic-co-glycolic) acid (PLGA) porogens, fast-resorbing glucono-delta-lactone (GDL) porogens, or mixtures thereof. The physicochemical, mechanical, and degradation characteristics of these CPC formulations were systematically analyzed upon soaking in phosphate-buffered saline (PBS). In parallel, various CPC formulations were implanted intramuscularly and orthotopically on top of the transverse process of goats followed by analysis of the soft tissue response and bone ingrowth after 12 weeks. In vitro degradation of GDL was almost completed after 2 weeks, as evidenced by characterization of the release of gluconic acid, while PLGA-containing CPCs released glycolic acid throughout the entire study (12 weeks), resulting in a decrease in compression strength of CPC. Extensive in vitro degradation of the CPC matrix was observed upon simultaneous incorporation of 30% PLGA-10% GDL. Histomorphometrical evaluation of the intramuscularly implanted samples revealed that all CPCs exhibited degradation, accompanied by an increase in capsule thickness. In the in vivo goat transverse process model, incorporation of 43% PLGA, 30% PLGA-5% GDL, and 30% PLGA-10% GDL in CPC significantly increased bone formation and resulted in higher bone height compared with both 10% GDL and 20% GDL-containing CPC samples.

A statistical approach to optimizing concrete mixture design.

A step-by-step statistical approach is proposed to obtain optimum proportioning of concrete mixtures using the data obtained through a statistically planned experimental program. The utility of the proposed approach for optimizing the design of concrete mixture is illustrated considering a typical case in which trial mixtures were considered according to a full factorial experiment design involving three factors and their three levels (3(3)). A total of 27 concrete mixtures with three replicates (81 specimens) were considered by varying the levels of key factors affecting compressive strength of concrete, namely, water/cementitious materials ratio (0.38, 0.43, and 0.48), cementitious materials content (350, 375, and 400 kg/m(3)), and fine/total aggregate ratio (0.35, 0.40, and 0.45). The experimental data were utilized to carry out analysis of variance (ANOVA) and to develop a polynomial regression model for compressive strength in terms of the three design factors considered in this study. The developed statistical model was used to show how optimization of concrete mixtures can be carried out with different possible options.

Electrospinning of PCL/PVP blends for tissue engineering scaffolds.

Currently, one of the main drawbacks of using poly(ε-caprolactone) in the biomedical and pharmaceutical fields is represented by its low biodegradation rate. To overcome this limitation, electrospinning of PCL blended with a water-soluble poly(N-vinyl-2-pyrrolidone) was used to fabricate scaffolds with tunable fiber surface morphology and controllable degradation rates. Electrospun scaffolds revealed a highly immiscible blend state. The incorporated PVP phase was dispersed as inclusions within the electrospun fibers, and then easily extracted by immersing them in cell culture medium, exhibiting nanoporosity on the fiber surface. As a striking result, nanoporosity facilitated not only fiber biodegradation rates, but also improved cell attachment and spreading on the blend electrospun scaffolds. The present findings demonstrate that simultaneous electrospinning technique for PCL with water-soluble PVP provides important insights for successful tuning biodegradation rate for the PCL electrospun scaffolds but not limited to expand other high valuable biocompatible polymers for the future biomedical applications, ranging from tissue regeneration to controlled drug delivery.

High-optical-quality blends of anionic polymethine salts and polycarbonate with enhanced third-order non-linearities for silicon-organic hybrid devices.

A series of anionic polymethine dyes with different aromatic counterions are prepared to improve their compatibility as guests in an amorphous polycarbonate host. When they are used as the cladding material for silicon hybrid slot waveguides, four-wave mixing wavelength conversion and two-photon absorption-based optical-power modulation are observed. Such guest-host materials may be attractive candidates for all-optical signal-processing applications.

Methods and options for the heterologous production of complex natural products.

This review will detail the motivations, experimental approaches, and growing list of successful cases associated with the heterologous production of complex natural products.

Effect of tricalcium aluminate on the properties of tricalcium silicate-tricalcium aluminate mixtures: setting time, mechanical strength and biocompatibility.

AIM: To prepare biphasic mixtures by adding Ca(3) Al(2) O(6) into Ca(3) SiO(5) and to evaluate the effect of Ca(3) Al(2) O(6) on physical and ex vivo biological properties of the Ca(3) SiO(5) /Ca(3) Al(2) O(6) mixtures derived from mineral trioxide aggregate (MTA). METHODOLOGY: Combinations of Ca(3) SiO(5) and Ca(3) Al(2) O(6) (0, 5%, 10% and 15%) powders were mixed with deionized water. After hydration, setting time, compressive strength, ex vivo bioactivity and biocompatibility of each mixture were investigated and compared to pure Ca(3) SiO(5) . RESULTS: With the addition of Ca(3) Al(2) O(6) from 0% to 15%, the initial setting time and final setting time of the Ca(3) SiO(5) /Ca(3) Al(2) O(6) mixtures decreased from 110 to 43min and from 220 to 97min, respectively (P≤0.05). However, the compressive strength increased from 6.75 to 16.20MPa after one day (P≤0.05) and from 17.73 to 29.13 Mpa after 28 days. Furthermore, the mixtures with 10% Ca(3) Al(2) O(6) or less had similar bioactivity and biocompatibility when compared to the pure Ca(3) SiO(5). CONCLUSIONS: The addition of Ca(3) Al(2) O(6) into Ca(3) SiO(5) accelerated the hydration process, reduced the setting time and improved the compressive strength. Furthermore, these mixtures were bioactive and biocompatible and had a stimulatory effect on the L929 cell growth when the content of Ca(3) Al(2) O(6) was below 10%. Therefore, the mixtures with 10% Ca(3) Al(2) O(6) produced the best compromise between hydration and ex vivo biological properties.

A VxD-based automatic blending system using multithreaded programming.

This paper discusses the object-oriented software design for an automatic blending system. By combining the advantages of a programmable logic controller (PLC) and an industrial control PC (ICPC), an automatic blending control system is developed for a chemical plant. The system structure and multithread-based communication approach are first presented in this paper. The overall software design issues, such as system requirements and functionalities, are then discussed in detail. Furthermore, by replacing the conventional dynamic link library (DLL) with virtual X device drivers (VxD's), a practical and cost-effective solution is provided to improve the robustness of the Windows platform-based automatic blending system in small- and medium-sized plants.

Molecular interactions in collagen and chitosan blends.

Molecular interactions between collagen and chitosan (CC) have the potential to produce biocomposites with novel properties. We have characterised the molecular interactions in CC complexes by viscometry, wide angle X-ray scattering and Fourier transform infrared spectroscopy. It was found that CC are miscible at the molecular level and exhibit interactions between the components; X-ray diffraction of CC blends indicate that the collagen helix structure is lost in CC films with increasing chitosan content. Non-linear viscometic behaviour with decreasing chitosan content is interpreted as evidence of a third structural phase formed as a complex of CC. The blending of collagen with chitosan gives the possibility of producing new bespoke materials for potential biomedical applications.

The effect of an admixture of sodium hydrogen phosphate or heparin-coating to poly(D,L)lactide--results of an animal study.

The study was aimed at investigating the effect of an admixture of sodium hydrogen phosphate (NaP) on the pH value around degrading poly(D,L)lactide (PDLLA) and the possible improvement of PDLLA biocompatibility by coating its surface with heparin. PDLLA +/- NaP was injection-molded to form rods (20 x 3 x 2 (mm)) and cubes (3 x 2 x 2 (mm)). Half of the pure PDLLA samples were surface-coated using heparin. One rod and cube each of PDLLA, PDLLA + NaP and PDLLA/Hep were implanted into the dorsal muscles of 42 rats. From the 2nd to 52nd week after operation, pH measurements were performed in the environment around the implants. The samples were then harvested for histological and mechanical analyses. No significant decrease in pH-values was observed in the tissue around the implants. Pure PDLLA and PDLLA/Hep samples were macroscopically resorbed after 52 weeks, while the degradation of PDLLA + NaP was still in progress. Approximately 80% of the initial bending strength of PDLLA or PDLLA/Hep rods was present after six weeks, while the bending strength of PDLLA + Nap was reduced to 50% after 4 weeks. Heparin-coating of PDLLA did not improve its biocompatibility but did increase its resorption. While no significant effect of NaP on pH value was found, its admixture did reduce the mechanical characteristics of the implants.