Application and Comparison of High-Speed Countercurrent Chromatography and High Performance Liquid Chromatography in Preparative Enantioseparation of α-Substitution Mandelic Acids

This paper is mainly about extending research on application and comparison of preparative high-speed countercurrent chromatography (HSCCC) and preparative high performance liquid chromatography (HPLC) in chiral separations. Preparative enantioseparations of α-cyclopentylmandelic acid and α-methylmandelic acid by HSCCC and HPLC were compared using hydroxypropy-β-cyclodextrin (HP-β-CD) and sulfobutyl ether-β-cyclodextrin (SBE-β-CD) as the chiral mobile phase additives. In preparative HPLC the enantioseparation was achieved on the ODS C₁₈ reverse phase column with the mobile phase composed of a mixture of acetonitrile and 0.10 mol L^?1 phosphate buffer at pH 2.68 containing 20 mmol L^?1 HP-β-CD for α-cyclopentylmandelic acid and 20 mmol L^?1 SBE-β-CD for α-methylmandelic acid. The maximum sample size for α-cyclopentylmandelic acid and α-methylmandelic acid was only about 10 mg and 5 mg, respectively. In preparative HSCCC the enantioseparations of these two racemates were performed with the two-phase solvent system composed of n-hexane-methyl tert.-butyl ether-0.1 molL^?1 phosphate buffer solution at pH 2.67 containing 0.1 mol L^?1 HP-β-CD for α-cyclopentylmandelic acid (8.5:1.5:10, v/v/v) and 0.1 mol L^?1 SBE-β-CD for α-methylmandelic acid (3:7:10, v/v/v). Under the optimum separation conditions, totally 250 mg of racemic α-cyclopentylmandelic acid could be completely enantioseparated by HSCCC with HP-β-CD as a chiral mobile phase additive in a single run, yielding 114-116 mg of enantiomers with 98-99% purity and 89-92% recovery. But, no complete enantioseparation of α-methylmandelic acid was achieved by preparative HSCCC with either of the chiral selectors due to their limited enantioselectivity. In this paper, preparative enantioseparation by HSCCC and HPLC was compared from various aspects.     

Using a β-Cyclodextrin-functional Fe3O4 as a Reinforcement of PLA: Synthesis,Thermal, and Combustion Properties

In this work, Fe₃O₄ nanoparticles were chemically grafted with β-cyclodextrin (β-CD@Fe₃O₄). Fe₃O₄ nanoparticles were modified using N,N-dimethylformamide as a solvent, β-cyclodextrin as a modifier, and 3-glycidoxypropyltrimethoxysilane as a coupling agent at room temperature. The obtained modified Fe₃O₄ were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, and thermogravimetric analysis techniques. β-CD@Fe₃O₄ was incorporated into a poly(lactic acid) matrix to prepare new green nanocomposites with modified properties. β-CD@Fe₃O₄ showed good dispersion in the poly(lactic acid) matrix and thermal and combustion properties of the nanocomposites were improved.     

Influences of Drying and Storage of Lycopene-Rich Carrots on the Carotenoid Content

ABSTRACT

The stability of β-carotene and lycopene was investigated during convective air and inert gas drying, microwave vacuum drying, and freeze-drying for lycopene containing carrots (Daucus carota L. cv. Nutri Red). After convection drying at temperatures below 70°C, β-carotene and lycopene contents remained unchanged independent of the drying medium. Freeze-drying did not show any advantage to convection-drying regarding carotenoid retention. Microwave vacuum–drying led to dry products with high carotenoid retention within very short drying times of about 2 h. Storage in air and in inert gas (nitrogen) containers was studied for convection-dried products, observing a better retention of carotenoids when using inert gas for a period of up to 6 months. After convection- and microwave vacuum–drying, an even better carotenoid extractability could be observed. No changes in the isomere fractions could be detected in any case.     

Morphological and Functional Expression of Fibroblast on Poly(lactide-co-glycolide)/β-Tricalcium Phosphate/Nature Bone

The in-vitro biocompatibility of degradable and bioactive composites consisting of poly(lactide-co-glycolide) (PLGA), β-tricalcium phosphate (β-TCP), and nature bone (NB) was investigated by culturing fibroblasts on the PLGA/β-TCP/NB substrates, and the cell morphology, proliferation, alkaline phosphatase (ALP) activity, and von Kossa mineralization were evaluated. The results showed that the incorporation of β-TCP and NB benefited fibroblasts attachment and the fibroblasts cultured on the PLGA/β-TCP/NB composite substrates spread better as compared to those on the pure PLGA after culturing for different times. MTT assay showed that the fibroblasts cultured on the PLGA/β-TCP/NB extraction revealed a higher proliferation rate than those on the pure PLGA extraction. ALP and von Kossa assay indicated that β-TCP and NB could promote biomineralization in vitro. All of the results showed that the addition of β-TCP and NB into PLGA could stimulate fibroblasts to proliferate and differentiate.     

Spray-Drying of α-Amylase—The Effect of Process Variables on the Enzyme Inactivation

ABSTRACT

The objective of this work was to investigate the effect of spray-drying conditions on the activity of enzyme and the process development. Several experiments were performed to determine the influence of the following variables: feed ratio speed and inlet and outlet drying air temperature. Fungal α-amylase was dissolved in a maltodextrin solution and spray-dried in a laboratory drier Anhydro. Water concentration and residual enzyme activity were determined in obtained powders as a function of the drying conditions. It was found that both temperature and feed ratio speed affected the activity retention of enzyme after drying. Higher value of feed ratio speed should be used in order to obtain high active dried α-amylase. Low outlet air temperature should be kept in order to obtain high active dried α-amylase.     

Evaluation of In-Vitro Cytotoxicity of Composite Materials Composed of Poly-L-lactic Acid and β-Tricalcium Phosphate

Composite material film composed of Poly-L-lactic acid (PLLA) and β-tricalcium phosphate (β-TCP) was prepared by a solvent evaporation technique. Cellular cultivation in vitro, Von Kossa staining and MTT assay were performed. The results of cytotoxicity test show that cells cultured in extracts of PLLA/β-TCP and on the surface of composite showed normal growth and proliferation, mineralization nodules were observed for fibroblasts cultured in PLLA/β-TCP extract at day 7. Compared with pure PLLA materials, β-TCP in the PLLA composite facilitate both adhesion and proliferation of rat fibroblasts on the PLLA/β-TCP composite film.     

Physicochemical Properties of Phytopharmaceutical Preparations as Affected by Drying Methods and Carriers

This article reports a study of the effects of the drying methods and drying carriers on system performance and physicochemical properties of spray- and spouted bed–dried phytopharmaceutical preparations from Bidens pilosa L. Colloidal silicon dioxide, β-cyclodextrin, maltodextrin dextrose equivalent (DE) 10, and microcrystalline cellulose were used as drying carriers. The dried product was characterized by the particle size and morphology, total flavonoid content, solubility, flowability, and water activity. High-performance liquid chromatography (HPLC) was used to detect four marker compounds previously reported for this plant. Spray and spouted bed drying systems were compared through energetic efficiency, product recovery, elutriation, and product accumulation. The crystalline state of the powders was assessed by X-ray diffraction. Results showed high degradation rates for total flavonoid content and marker compounds during spouted bed drying. Depending on the drying carrier added to extractive solutions, different degrees of protection from degradation were conferred, and the physical characteristics of the product were changed accordingly. The lowest flavonoid degradation (8.6%) and the higher concentration of marker compounds were obtained using β-cyclodextrin as the drying carrier. Particle size was higher when a blend of Aerosil (Evonik Degussa, Hanau, Germany) and cellulose was employed as the drying carrier. A maximum product recovery of 86.9% was achieved by spray drying and 72.9% by spouted bed drying with the Aerosil : cellulose composition.     

The Relationship Between the Microhardness and Glass Transition Temperature of Inorganic Glasses Compared with Polymeric Glasses

ABSTRACT

In this article an attempt is undertaken to verify the approach already successfully applied to polymeric glasses for deriving a simple analytic relationship between the glass transition temperature, T_g , and Vickers microhardness, H_v , (for polymers it is H_v  = 1.57 T_g –571, H_v in MPa, T_g in K). On the basis of previously reported data for H_v and T_g of 12 inorganic glasses (lead-silicate-, alkali-silicate-, alumosilacate, and quartz glasses) a linear relationship in the form H_v  = 5.87 T _g + 1740 (H_v in MPa, T_g in K) is derived. In addition, a critical analysis of the published attempt for theoretical deriving of the relationship between H_v and T_g is also offered.     

Suppression of β-crystal in iPP/PET Fiber Composites

The β-crystal formed in PP/PET fiber composites was investigated. The results indicate that PET fibers (PF) can preferably lead to α-crystal formation on their surface. Besides, α-crystals occur earlier than those in the bulk. The β-crystal, might be induced by temperature gradient, only formed away from the PF in composites with lower content of PF. The higher the content of PF is, more possible the PF network is constructed. The transcrystallinity induced by PF will rapidly occupy the region between the adjacent PFs. Consequently, owing to the spatial confinement, β-form is suppressed in the composites with higher content of PF.     

Extraction and Separation of α-lactalbumin and β-Lactoglobulin from Skim Milk by Microfiltration and Ultrafiltration at High Shear Rates: A Feasibility Study

Abstract

This paper presents a two-stage membrane filtration process for extracting and separating α-Lactalbumin (α-La) and β-Lactoglobulin (β-Lg), from UHT skim milk, using dynamic filtration. The 1st stage separates casein micelles in retentate from whey proteins in the permeate with rotating 0.2 µm pores ceramic membrane disks. Casein micelles rejection was excellent, while α-La and β-Lg transmissions remained between 80 and 90%. The permeate flux at 40°C ranged from 105 to 40 Lh^?1m^?2 at a volume reduction ratio of VRR = 4. The 2nd stage consisted of ultrafiltration of the previous permeate with a metal disk rotating at 2000 rpm near a fixed 50 kDa PES membrane, in order to concentrate β-Lg in retentate, while collecting α-La in the permeate. The flux dropped from 270 Lh^?1m^?2 at VRR = 1, and remained nearly constant at 200 Lh^?1m^?2 until a VRR of 3.3. α-La transmission increased with VRR to reach 23% at VRR = 3.3, while β-Lg transmission decayed at increasing VRR to 3%, to give a maximum selectivity of 8.     

Influence of β-Nucleators on iPP Crystallization and Morphology

In this article, the effects of the β-nucleators WBG and WOT on the crystallization behavior and morphology of isotactic polypropylene (iPP) were investigated using a combination of differential scanning calorimetry (DSC), wide-angle X-ray (WAXD), polarized optical microscopy (POM) and atomic force microscopy (AFM). The results showed that the amount of β-form and the spherulite size decreased with increasing WBG contents. At about 0.15 wt. % WBG nucleator, the formation of the β-form was evidently observed. Whereas, for the iPP with low content of WOT nucleator, the formation of the β-form was almost the same as that of pure iPP.     

Effect of Different Drying Methods and 24-Month Storage on Water Activity,Rehydration Capacity,and Antioxidants in Boletus edulis Mushrooms

This article evaluates the effect of air drying, freeze drying, and 24-month storage at 4 and 20 ^° C on unblanched and blanched Boletus edulis . Water content and activity were lower in freeze-dried mushrooms than in air-dried mushrooms, whereas rehydration capacity showed the opposite tendency. Drying resulted in substantial losses of the following antioxidants: total flavonoids (4–7%), vitamin C (2–36%), β-carotene (26–32%), and total tocopherols (72–81%); total polyphenols increased during air drying (7–17%) and decreased during freeze drying (5–7%). Antioxidant activity increased 1–33% during drying. Storage led to further changes in the quality of dried mushrooms. After 24 months, no vitamin C or tocopherols were detected, and water content and activity were moderately high.     

Kinetic Models of β-Carotene Degradation During Air Drying of Carrots

The objective of this study was to determine the kinetic parameters of models that describe the joint influence of temperature and moisture content on the thermal degradation of β-carotene in a drying process of carrots. Two models were used: a first-order decay model with an Arrhenius and a polynomial dependency on temperature and water content, respectively, and a decay model with a WLF dependency of the decimal reduction time on glass transition temperature (Tg), with the Gordon and Taylor equation describing the influence of moisture content on Tg. Carrots were dehydrated in a cabinet air dryer at 50, 60, 70, and 80°C. Carrot samples were drawn at 20-min intervals and analyzed for moisture and β-carotene content. The parameters of the two models were estimated by nonlinear regression. In addition, the models were evaluated by comparing their predictions and experimental data during drying at 80°C of carrot slices with thickness of 3, 6, and 9 mm. Both models were found suitable for modeling the β-carotene degradation, though the lower sum of squares of residuals (SSQ) of the Tg approach model and the similar WLF parameters calculated at different drying air temperatures demonstrated the higher predictive ability of the Tg model over the more common empirical dependence model.     

Structures and Performance of White Clay-Filled Isotactic-Polypropylene Composites Prepared by Double-Molding Techniques

Various contents of Bangladeshi white clay (WC)-filled Isotactic polypropylene (iPP) composites were fabricated by double-molding techniques. Scanning electron micrographs shows a good impact between iPP matrix and fillers. X-diffraction and IR spectroscopic measurements reveal that inclusion of fillers develops an additional γ-crystal along with the α- and β-crystals that are merely observed in the neat iPP. Young's modulus and microhardness are found to increase with increasing WC content. Thermal analyses represent a considerable increase of thermal stability of the composites with filler addition. Appearance of new crystalline phase by filler inclusion and performances of the composites are discussed in detail.     

Studies on the Preparation of Polystyrene Thermal Conductivity Composites

Various thermally conductive fillers including aluminum oxide(Al₂O₃), magnesium oxide(MgO), β-silicon carbide particle(β-SiCp) and β-silicon carbide whisker(β-SiCw) were used to prepare polystyrene thermal conductivity composites. Experimental results showed that, for given filler loading, the thermal conductivity of the composites was higher for PS flake than that of PS particle, and the thermal conductivity was optimal by powder blending method. The SiCw filler was more favorable to improve the thermal conductivity of the composites; a much higher thermal conductivity of 1.18 W/mK could be achieved for the composite with 40 vol% SiCw, about six times higher than that of native polystyrene. The experimental thermal conductivity values were in agreement with those predicted by lower bound of Maxwell-Eueken model. For given SiC loading, the thermal conductivity increased with the increasing shape parameter of n. The SiCw was much easier to form the thermal conductivity chains and network than that of SiCp.     

Effect of Calcium Salts of Glutaric Acid and Pimelic Acid on the Formation of β Crystalline Form in Isotactic Polypropylene

The effect of calcium glutarate (Cagt) and calcium pimelate (Capt) on the formation of β crystalline form in isotactic polypropylene (iPP) after isothermal crystallization at 130°C for 30 min has been investigated. The maximum K_WAXD and K_DSC values were 31.97% and 38.06%, respectively, for iPP doped with 0.2 wt.% Cagt. The maximum values of K_WAXD and K_DSC were 73.60% and 68.44% for iPP doped with 0.3 wt.% and 0.15 wt.% Capt, respectively. The crystal size of iPP doped with Capt is finer than that of iPP doped with Cagt. It is shown that the β nucleation ability of Capt is superior to that of Cagt. The difference in the β nucleation ability between Cagt and Capt is explained by the structural difference of the nucleators with β-iPP.     

Microencapsulation of Gac Oil by Spray Drying: Optimization of Wall Material Concentration and Oil Load Using Response Surface Methodology

The objective of this study was to optimize the wall material concentration and the oil load on the encapsulation of Gac oil using spray drying by response surface methodology. Results showed that the quadratic polynomial model was sufficient to describe and predict encapsulation efficiencies in terms of oil, β-carotene, lycopene, peroxide value (PV), moisture content (MC), and total color difference (Δ E) with R ² values of 0.96, 0.95, 0.86, 0.89, 0.88, and 0.87, respectively. Under optimum conditions (wall concentration of 29.5 % and oil load of 0.2), the encapsulation efficiencies for oil, β-carotene, lycopene, PV, MC, and Δ E were predicted and confirmed as 92 %, 80 %, 74 %, 3.91 meq/kg, 4.14 % and 12.38, respectively. The physical properties of the encapsulated oil powders obtained by different formulations were also determined. It was concluded that the protein-polysaccharide matrix as the wall material was effectively used for spray-drying encapsulation of Gac oil.     

RELEASE OF β-GALACTOSIDASE FROM INDIGENOUS LACTOBACILLUS ACIDOPHILUS BY ULTRASONICATION: PROCESS OPTIMIZATION

Lactobacillus acidophilus isolated indigenously from Eleusine coracana has been reported by us to be a good producer of β-galactosidase (Akolkar et al., 2005 Akolkar , S. K. , Sajgure , A. , and Lele , S. S. ( 2005 ). Lactase production from Lactobacillus acidophilus , World J. Microbiol. Biotechnol. , 21 , 1119 – 1122 .[Crossref], [Web of Science ®] , [Google Scholar]). Recovery of this intracellular enzyme using ultrasonication was found to be the rate-limiting step for subsequent downstream processing. Among the various chemical and mechanical methods tried, ultrasonication was found to be the most effective. However, prolonged ultrasonication can result in partial to complete degradation of the released enzyme. This article reports the optimization of the ultrasonication process for release of β-galactosidase using response surface methodology (RSM). Factors like cell density, sample volume, and ultrasonication time, which were critical for the release of the enzyme at a constant acoustic power, were considered in the optimization to develop an efficient release process. Increase in the release of β-galactosidase from 320 U/gm DCW to 483 ± 1.9 U/gm DCW was achieved at the optimized ultrasonic process conditions (cell density 2.1% wet weight, suspension volume 11 mL, and ultrasonication time 15 min) at a constant acoustic power of 50 W.     

Influence of Different Solvents on the Morphology of the Hybrid Layer Using Two-Step Etch-and-Rinse Adhesives

To evaluate if different etch-and-rinse adhesive solvents influenced the hybrid layer's morphology.

Four one-bottle etch-and-rinse adhesive systems containing different solvents—Group A: Scotchbond 1XT?– 3 M ESPE, Group B: XP – Bond? – Dentsply, Group C: Prime&;Bond NT® – Dentply, and Group D: One Coat Bond® - Coltène Whaledent—were applied onto 32 dentin discs which were thermocycled, prepared, and examined using field-emission scanning electron microscopy. Micrographs were scanned and the data were processed using Statistical Package for Social Sciences. The mean value and standard deviation were calculated and the Anova Multivariant Test was used.

The hybrid layer thickness average found was 3.23 µm (±0.53) in Group A, 3.13 µm (±0.73) in Group B, 2.53 µm (±0.50) in Group C, and 1.84 µm (±0.27) in Group D. Prime&;Bond NT® presented a more inconsistent hybrid layer.

The solvent seems to play a significant role in hybrid layer structure and thickness.     

Effect of Microstructure of EPR on Crystallization and Morphology of PP/EPR Blends

Two ethylene-propylene random copolymer (EPR) fractions (sol-EPR: soluble part and insol-EPR: insoluble part in n-octane) were blended with polypropylene (PP). It was found hat sol-EPR has a random sequence distribution and is nearly amorphous, whereas insol-EPR contains long ethylene and propylene sequences and is partially crystalline. The crystallization and melting behaviors, linear spherulitic growth rate, crystal structure, and morphology were investigated with differential scanning calorimetry, polarized optical microscopy, wide angle X-ray diffraction, and scanning electron microscopy. It was observed that the PP/insol-EPR blends have a smaller domain size of EPR and a rougher fracture surface. The better compatibility between insol-EPR and PP leads to lower melting temperature (T _m) of PP/insol-EPR blends than the neat PP. For the blends cooled in air from the melt, both α and β crystals were observed. At low weight fraction (0–10%), EPR enhances the relative content of β crystals. When the weight fraction of EPR exceeds 10%, sol-EPR and insol-EPR decrease the relative content of β crystals in the blends to different extents. This difference can be correlated to the fact that sol-EPR and insol-EPR reduce the linear spherulitic growth rate (G) of PP to different extents.