Preparation of high surface area mesoporous nickel oxides and catalytic oxidation of toluene and formaldehyde

Mesoporous nickel oxide (NiO) nanoparticles were synthesized by the thermal decomposition reaction of Ni(NO₃)₂·9H₂O using oxalic acid dihydrate as the mesoporous template reagent. The pore structure of nanocrystals could be controlled by the precursor to oxalic acid dihydrate molar ratio, thermal decomposition temperature and thermal decomposition time. The structural characteristic and textural properties of resultant nickel oxide nanocrytals were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N₂ adsorption–desorption isotherm and temperature programmed reduction. The results showed that the most excellently mesoporous nickel oxide particles (m-Ni-1-4) with developed wormlike pores were prepared under the conditions of the mixed equimolar precursor and oxalic acid and calcined for 4 h at 400 °C. The specific surface area and pore volume of m-Ni-1-4 are 236 m² g^?1 and 0.42 cm³ g^?1, respectively. Over m-Ni-1-4 at space velocity = 20,000 mL g^?1 h^?1, the conversions of toluene and formaldehyde achieved 90 % at 242 and 160 °C, respectively. It is concluded that the reactant thermal decomposition with oxalic acid assist is a key step to improve the mesoporous quality of the nickel oxide materials, the developed mesoporous architecture, high surface area, low temperature reducibility and coexistence of multiple oxidation state nickel species for the excellent catalytic performance of m-Ni-1-4.     

Novel amphiphilic temperature responsive graft copolymers PCL-<Emphasis Type="Italic">g</Emphasis>-P(MEO<Subscript>2</Subscript>MA-<Emphasis Type="Italic">co</Emphasis>-OEGMA) via a combination of ROP and ATRP: synthesis,characterization, and sol-gel transition

A series of well-defined novel amphiphilic temperature-responsive graft copolymers containing PCL analogues P(αClεCL-co-εCL) as the hydrophobic backbone, and the hydrophilic side-chain PEG analogues P(MEO₂MA-co-OEGMA), designated as P(αClεCL-co-εCL)-g-P(MEO₂MA-co-OEGMA) have been prepared via a combination of ring-opening polymerization (ROP) and atom transfer radical polymerization (ATRP). The composition and structure of these copolymers were characterized by ¹H NMR and GPC analyses. The self-assembly behaviors of these amphiphilic graft copolymers were investigated by UV transmittance, a fluorescence probe method, dynamic light scattering (DLS) and transmission electron microscopy (TEM) analyses. The results showed that the graft copolymers exhibited the good solubility in water, and was given the low critical temperature (LCST) at 35(±1) °C, which closed to human physiological temperature. The critical micelle concentrations (CMC) of P(αClεCL-co-εCL)-g-P(MEO₂MA-co-OEGMA) in aqueous solution were investigated to be 2.0 × 10^?3, 9.1 × 10^?4 and 1.5 × 10^?3 mg·mL^?1, respectively. The copolymer could self-assemble into sphere-like aggregates in aqueous solution with diverse sizes when changing the environmental temperature. The vial inversion test demonstrated that the graft copolymers could trigger the sol-gel transition which also depended on the temperature.     

Production of MLM-Type Structured Lipids Catalyzed by Immobilized Heterologous <Emphasis Type="Italic">Rhizopus oryzae</Emphasis> Lipase

This work aims to produce triacylglycerols (TAG) containing a medium-chain fatty acid (M) at positions sn-1,3 and a long-chain fatty acid (L) at sn-2 position, i.e. TAG of MLM type, by acidolysis of virgin olive oil with caprylic (C8:0) or capric (C10:0) acids, catalyzed by 1,3-selective Rhizopus oryzae heterologous lipase (rROL) immobilized in Eupergit^® C and modified sepiolite. This lipase was produced by the methylotrophic yeast Pichia pastoris. Reactions were performed at 25 and 40 °C, for 24 h, either in solvent-free or in n-hexane media, at a molar ratio 1:2 (olive oil:free fatty acid). Higher incorporations of C8:0 (21.6 mol%) and C10:0 (34.8 mol%) into the TAG were attained in solvent-free media, at 40 °C, when rROL immobilized in Eupergit^® C was used. In organic media, at 40 °C, only 15.9 and 14.1 mol%, incorporation of C8:0 or C10:0 were, respectively observed. Lower incorporations were attained for both acids (3.4–7.0 mol%) when native ROL (nROL) in both supports and rROL in modified sepiolite were used. rROL in Eupergit^® C maintained its activity during the first four or three 23-h batches, respectively when C8:0 (half-life time, t _1/2 = 159 h) or C10:0 (t _1/2 = 136 h) were used, decreasing thereafter following a time delay model.     

Effect of epoxidized soybean oil grafted poly(12-hydroxy stearate) on mechanical and thermal properties of microcrystalline cellulose fibers/polypropylene composites

A new green compatibilizer named epoxidized soybean oil grafted poly(12-hydroxy stearate) (ESO-g-PHS) was successfully synthesized using 12-hydroxy stearic acid and epoxidized soybean oil (ESO). The chemical structure of ESO-g-PHS was investigated through Fourier transformed infrared spectroscopy, thermogravimetric analysis, and gel permeation chromatography. ESO-g-PHS was used as a compatibilizer to enhance the interfacial compatibility between polypropylene (PP) and microcrystalline cellulose fibers (MCF). The results showed that the impact strength and tensile strength were 33.55 and 27.57 MPa when the content loading of MCF reached 10 wt% and ESO-g-PHS was 4 wt%, which enhanced by 75.4 and 30.04 %, respectively, compared to that of composites without ESO-g-PHS. In addition, the SEM images of the fracture surfaces display that PP was highly bonded to MCF with ESO-g-PHS treated. In addition, the wide angle X-ray diffraction measurement revealed that the addition of ESO-g-PHS did not change the crystal structure of PP. Moreover, there was a slight improvement in thermal properties for PP composites with the addition of ESO-g-PHS.     

Synthesis and characterization of polyimides from 4,4′-(3-(<Emphasis Type="Italic">tert</Emphasis>-butyl)-4-aminophenoxy)diphenyl ether

A novel diamine 4,4′-(3-(tert-butyl)-4-aminophenoxy)diphenyl ether (4) was synthesized from 2-tert-butylaniline and 4,4′-oxydiphenol through iodination, acetyl protection, coupling reaction and deacetylation protection. Then some polyimides (PIs) were obtained by one-pot polycondensation of diamne 4 with several commercial aromatic dianhydrides respectively. They all exhibit enhanced solubility in organic solvents (such as NMP, DMF, THF and CHCl₃ etc.) at room temperature. Their number-average molecular weights are in the range of (2.1–3.7)?×?10⁴ g/mol with PDI from 2.25 to 2.74 by GPC. They can form transparent, tough and flexible films by solution-casting. The light transparency of them is higher than 90% in the visible light range from 400 nm to 760 nm and the cut-off wavelengths of UV–vis absorption are below 370 nm. They also display the outstanding thermal stability with the 5% weight loss temperature from 525 °C to 529 °C in nitrogen atmosphere. The glass transition temperatures (T _g s) are higher than 264 °C by DSC. XRD results demonstrate that these PIs are amorphous polymers with the lower water absorption (<0.66%). In summary, the incorporation of tert-butyl groups and multiple phenoxy units into the rigid PI backbones can endow them excellent solubility and transparency with relatively high T _g s.     

Synthesis,Structures, and Catalytic Properties of Two Zinc(II) Coordination Polymers Constructed from Polycarboxylate and Bis(Benzimidazole) Ligands

Two Zn(II) coordination polymers, formulated as {[Zn(L1)_0.5(btc)_0.5(H₂O)]·H₂O} _n (1) and {[Zn(L2)(1,4-ndc)]·2H₂O} _n (2) [L1 = 1,4-bis(2-methylbenzimidazole-1-ylmethyl)benzene, L2 = 1,4-bis(2-methylbenzimidazole)butane, H₄btc = butane-1,2,3,4-tetracarboxylic acid, 1,4-H₂ndc = 1,4-naphthalenedicarboxylic acid] have been synthesized and structurally characterized by single crystal X-ray diffraction. Complex 1 features a 3D (3,4)-connected network with the topology of fsh-3,4-P2₁/c. Complex 2 is a 2D (4,4) grid with sql topology and further extends into a 3D supramolecular framework by π–π stacking interactions. In addition, the thermal stability, fluorescence, and catalytic properties of two complexes for degrading methyl orange dye in a Fenton-like process were investigated.     

Production of Saponin Biosurfactant from <Emphasis Type="Italic">Glycyrrhiza glabra</Emphasis> as an Agent for Upgrading Heavy Crude Oil

Saponins are the main group of phytogenic biosurfactants extracted from plants. One of the significant applications of these compounds is upgrading and viscosity reduction of heavy crude oil water in oil (W/O) emulsions. In this research, use of saponin extracted from Glycyrrhiza glabra was investigated for viscosity reduction of heavy crude oil and upgrading its API properties. The extracted saponin was characterized using Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy. Phase behavior analysis demonstrated a reduction in initial viscosity and improved API gravity of the heavy oil from 2350 mPa·s and 19 to 900 mPa·s and 27, respectively. In addition, the emulsification index (E ₂₄) was found to be 98 % at a saponin concentration of 8 % w/v. It was observed that the emulsions were stable in the pH range of 5.5–13, temperature from 30 to 80 °C and salinity up to 6 % w/v of NaCl solution. Average diameter of W/O droplets evaluated by dynamic light scattering (DLS) were in the range of 10–15 µm. The results obtained from the present research revealed that the extracted saponin improved the physical characteristics of heavy crude oil. We propose the use of saponin as a potential alternative to conventional emulsifiers for upgrading heavy crude oil in petroleum industry.     

Medium-Chain Enriched Diacylglycerol (MCE-DAG) Oil Decreases Body Fat Mass in Mice by Increasing Lipolysis and Thermogenesis in Adipose Tissue

Medium chain fatty acid (MCFA) escapes the formation of chylomicrons in the small intestine, resulting in energy expenditure through beta-oxidation. Diacylglycerol (DAG) is susceptible to oxidation rather than being stored in the adipose tissue. This study was conducted to verify the effect of MCE-DAG oil on body fat mass in vivo. Male C57BL/6 mice were randomly assigned to four groups (n = 12) as follows: (1) normal diet (18% kcal from fat), (2) canola oil as a control (40% kcal from canola oil), (3) MCE-DAG10 (10% kcal from MCE-DAG + 30% kcal from canola oil), and (4) MCE-DAG20 (20% kcal from MCE-DAG + 20% kcal from canola oil). The body weight and fat mass of MCE-DAG20 group mice were decreased relative to those of control mice (P < 0.05 and P < 0.001, respectively). Serum triacylglycerol (TAG) was decreased in both MCE-DAG10 and MCE-DAG20 groups (P < 0.01 and P < 0.05, respectively). Hormone sensitive lipase (HSL) and adipose triglyceride lipase (ATGL) were increased in the MCE-DAG20 group relative to the control in white adipose tissue (WAT) (P < 0.05). Uncoupling protein 1 (UCP1) was also increased in the MCE-DAG20 group relative to the control in brown adipose tissue (BAT) (P < 0.05). In summary, MCE-DAG reduced body fat mass likely by stimulating lipolysis in WAT and thermogenesis in BAT.     

Sol-Gel Synthesis,Thermal Behavior of Nanopowders and Chemical Stability of La<Subscript>1 – <Emphasis Type="Italic">x</Emphasis></Subscript>Ho<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>PO<Subscript>4</Subscript> Ceramic Matrices

Nanosized powders of orthophosphates in the LaPO₄–HoPO₄–H₂O system have been synthesized to determine the mutual solubility of LaPO₄ · nH₂O and HoPO₄ · nH₂O initial components and to obtain ceramic matrices by sintering them. Formation of hexagonal, monoclinic or tetragonal solid solutions was revealed, and their limits and thermal stability were determined. A series of limited hexagonal LaPO₄ · nH₂O-based solid solutions was observed within the 0 ≤ x ≤ 0.6 concentration range up to 600°C. Further they transformed to monoclinic LaPO₄-based form within the 0 ≤ x ≤ 0.3 concentration range. Solubility of LaPO₄ · nH₂O and LaPO₄ in tetragonal HoPO₄(· nH₂O) is lower (≤10 mol %). Specific surface area of La_1–xHo_xPO₄ · nH₂O powders was in the range of 90.5–165.0 m²/g depending on x. Leaching rate of La³⁺ and Ho³⁺ from La_1–xHo_xPO₄ matrices in nitric acid solution (pH 1–2) was determined to be 10^–5–10^–2 g/(cm² day) for both ions.     

Syntheses and Characterization of Three Coordination Polymers of Zinc(II) and Cadmium(II) with Dicarboxylates and Bis(thiabendazole) Ligands

Three d ¹⁰ coordination polymers formulated as [Zn(L1)₂(mip)] _n (1), [Zn(L1)(2,6-ndc)] _n (2) and [Cd(L2)_0.5(bpdc)] _n (3) (L1 = 1,1′-(1,3-propanediyl)bis(thiabendazole), L2 = 1,1′-(1,6-hexanediyl)bis(thiabendazole), H₂mip = 5-methylisophthalic acid, 2,6-H₂ndc = 2,6-naphthalenedicarboxylic acid, H₂bpdc = 4,4′-biphenyldicarboxylic acid) were hydrothermally synthesized. Complexes 1–3 were characterized by elemental analysis, IR spectroscopy, X-ray powder diffraction analysis, and single crystal X-ray diffraction. Complexes 1 and 2 present different chain structures, both of them are extended into 2D supramolecular architectures via C–H···O hydrogen bonds, while 3 is a three-fold interpenetrating three-dimensional framework with binodal 4,4-connected mog topology. The thermal stability, UV–visible spectroscopy and luminescence properties of complexes 1–3 were also examined. Furthermore, complex 3 exhibits relatively positive catalytic activity towards the degradation of methyl orange in a Fenton-like process.     

Gas Chromatographic Separation and Identification of Jacaric and Punicic 2-Ethyl-1-Hexyl Esters

The present study demonstrates the separation of a critical pair of conjugated linolenic acid (CLN) isomers—jacaric acid (JA; c8, t10, c12-18:3) and punicic acid (PA; c9, t11, c13-18:3)—on a 60-m conventional Supelcowax 10 column. The alkyl esters of different alcohols (C₁–C₈) of JA and PA were prepared and analyzed isothermally at 220, 230 and 240 °C. The adequacy of their separation was determined from the separation factors (α) and peak resolutions (R _s). Acceptable resolution (R _s = 1.01) of JA and PA was obtained with their 2-ethyl-1-hexyl ester derivatives at a column temperature of 230 °C. In addition, the Gibbs energy of transfer from solution to gas of the three double bonds \((\Delta_{\text{sln}}^{\text{g}} G_{\text{u}}\)) could be used to describe the interactions of the double bond with the stationary phase. Characterization of 2-ethyl-1-hexyl esters of Jacaranda mimosifolia seed oil at 230 °C demonstrates that the oil contains JA and α- and β-calendic acid as a CLN without the presence of PA. The results suggested that JA could be resolved from PA on a 60-m Supelcowax 10 column as the ethyl hexyl ester.     

Preparation,Infra-red,MAS-NMR and Structural Characterization of a New Copper Based Inorganic–Organic Hybrid Compound: [C<Subscript>5</Subscript>H<Subscript>6</Subscript>N<Subscript>2</Subscript>Cl]<Subscript>2</Subscript>CuCl<Subscript>4</Subscript>

The ionic salt [2(C₅H₆N₂Cl)⁺], [CuCl₄]^2? complex of copper(II) has been synthesized and characterized. The X-ray diffraction analysis with a single crystal of this compound showed that the title compound (4-amino-2-chloropyridinium)₂CuCl₄ [(CAP)₂CuCl₄], crystallized at room temperature in the monoclinic system, space group C_2/c (N°.15) and the following : a = 16.0064 (2) Å; b = 7.7964 (10) Å; c = 14.7240 (2) Å; β = 102.497 (10)°; V = 1793.91 (4) ų and Z = 4. The structure was solved by using 1,589 independent reflections down to R value of 0.021. The unit cell is made up of tetrachlorocuprate(II) anions and 4-amino-2-chloropyridinium cations linked together by an extensive hydrogen bond network of types N–H···Cl (N: pyridinium) and N–H···Cl (N: amine), and cation-lone pair of nitrogen element interactions. Solid state NMR spectra showed one and five isotropic resonances, ⁶³Cu and ¹³C, respectively, confirming the solid state structure determined by X-ray diffraction. Impedance spectroscopy study, reported for single crystal, revealed that the conduction in the material was due to a hopping process. This work aims to reveal the thermal properties of a new copper(II) based organic–inorganic hybrid and the conductivity properties that these compounds exhibit.     

Partition of <Emphasis Type="Italic">n</Emphasis>-Butanol Among Phases and Solubilization Ability of Winsor type III Microemulsions

The partition of n-butanol in Winsor type III (W-III) microemulsions was investigated in this work. Three kinds of anionic surfactants (sodium dodecyl sulfate (SDS), sodium dodecyl sulfonate (DSS), and sodium dodecyl benzene sulfonate (SDBS)) and two kinds of anionic/cationic surfactant mixtures (SDS/octadecyl trimethyl ammonium chloride (OTAC) mixtures and DSS/OTAC mixtures) were studied. Internal standard gas chromatography was employed in n-butanol content analysis. The results showed that no water exists in the excess oil (EO) phase and no oil exists in the excess water (EW) phase. For the W-III microemulsions obtained by salinity scanning, relatively constant n-butanol content in the EO (11–12 v%) and EW (1–4 v%) was found under different salinities. Accurate measurement of n-butanol content in each phase is important for those systems having low solubilization ability. For the W-III microemulsions prepared using SDS/OTAC surfactant mixture, the percentage of n-butanol distributed into the interfacial layer decreased while the fraction of n-butanol in the interfacial layer first increased sharply and then tended to be stable with the addition of n-butanol. For the different optimum W-III microemulsion systems tested, most of the surfactant-to-alcohol molar ratio data are near 1:3, but obvious deviation could be observed for some data. On the basis of the accurate measurement of n-butanol content in the EO and EW phases, the standard free energy, ΔG _o→in ^* (T = 298.15 K) of n-butanol transferring from the EO phase to the interfacial region was calculated. The results show negative ΔG _o→in ^* values. For microemulsions with the same components, n-butanol content is an important factor influencing the ΔG _o→in ^* value, and a high absolute value of ΔG _o→in ^* leads to high solubilization ability.     

Tocopherols,Tocotrienols and Carotenoids in Kernel Oils Recovered from 15 Apricot (<Emphasis Type="Italic">Prunus armeniaca</Emphasis> L.) Genotypes

We studied the content of tocopherols, tocotrienols and carotenoids in oil extracted from the kernels of 15 apricot (Prunus armeniaca L.) genotypes and the associated oil yield of the studied samples. The oil yield in apricot kernels was in a wide range of 27.2–61.4% (w/w) dry weight basis. For each class of studied compounds (tocochromanols and carotenoids), a three-fold difference was found between the lowest and the highest content (78.8–258.5 and 0.15–0.53 mg/100 g of oil, respectively). γ-Tocopherol accounted for 91–94% of total tocochromanols detected in all tested samples. Lutein, zeaxanthin, β-cryptoxanthin and β-carotene were the main compounds among the eight different carotenoids detected in apricot kernel oils; they comprised 76–94% of the total carotenoids content, and compositions were characteristic for specific genotypes. The oil yield and content of lipophilic antioxidants in apricot kernel oils were significantly affected by the genotype. The oil yield was negatively correlated with the total amount of tocochromanols (r = ?0.910) and carotenoids (r = ?0.704) in apricot kernel oils.     

Some properties of xanthan gum in aqueous solutions: effect of temperature and pH

The properties of xanthan gum (XG) aqueous solutions were investigated by using viscometric, electrokinetic and surface tension measurements. The effects of polymer concentration, temperature and pH on the viscosity of the XG solutions were evaluated and discussed. Zeta potential data determined for XG solutions in water in the temperature range of 15–45 °C corroborated with the results obtained from the viscometric investigations suggest the occurence of conformational changes above 36 °C. The activation energy of flow and that associated with the electrophoretic migration of the charged particles were estimated for XG solutions in water. In acid medium, xanthan gum determines a slight decrease of the surface tension of pure water at all investigated temperatures.     

Efficient and Reusable Pb(II) Metal–Organic Framework for Knoevenagel Condensation

A microporous lead–organic framework {[Pb₄(µ₈-MTB)₂(H₂O)₄]·5DMF·H₂O}_n (MTB?=?methanetetrabenzoate, DMF?=?N,N′-dimethylformamide) was synthesized and studied as a catalyst in Knoevenagel condensation reactions. The framework is built from tetranuclear [Pb₄(µ₃-COO)(µ₂-COO)₆(COO)(H₂O)₄] clusters and exhibits a 3D structure, with repeated 1D jar-like cavities with sizes about 14.98?×?7.88 and 14.98?×?13.17 Å² and BET specific surface area of 980 m² g^?1. To obtain open framework with unsaturated Pb(II) sites needed for catalysis, the thermal activation of the solvent exchanged sample was performed (DMF was exchanged by EtOH). The activated compound was tested in Knoevenagel condensation of bulky aldehydes and active methylene compounds at different temperatures. Excellent catalytic conversion and selectivity in condensation of small-sized aldehydes with malononitrile was observed, which indicates that the opened Pb(II) sites play a significant role in the heterogeneous catalytic process. Leaching test confirmed the stability of the catalyst in catalytic reactions. Moreover, the compound displayed good recyclability after several reuses without significant decrease in the original catalytic activity.

Graphical Abstract

Novel Pb(II) metal–organic framework was tested in Knoevenagel condensation. The catalyst showed excellent catalytic conversion, selectivity and recyclability. Aldehydes with lower kinetic diameter demonstrated high conversions and yields. Catalyst is less efficient for condensation of larger aromatic aldehydes.

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Synthesis and Characterization of pH-Responsive Organic–Inorganic Hybrid Material with Excellent Catalytic Activity

Poly(N-isopropylmethacrylamide-co-methacrylic acid) [p(NipAam-Mac)] microgels were synthesized and used as microreactors to fabricate silver nanoparticles. Pure and hybrid microgels were characterized using Ultraviolet–Visible (UV/Vis) spectroscopy, Fourier transform infra-red (FTIR) spectroscopy and transmission electron microscopy (TEM). Catalytic activity of hybrid microgels and mechanism of catalysis by this system was explored using different reaction conditions. At the same temperature, apparent rate constant (k_app) was found to be varied from 0.0414 to 0.7852 min^?1 by increasing the concentration of NaBH₄ from 2.49 to 22.41 mM at constant concentration of substrate and catalyst. However upon extra increase in concentration of NaBH₄ from 22.41 to 37.35 mM reduced the value of k_app to 0.2178 min^?1. Likewise, the value of k_app was found to be increased from 0.1242 to 0.5495 min^?1 with increasing the concentration of 4-nitrophenol [Para-nitrophenol (p-Np)] from 0.063 to 0.079 mM keeping other parameters constant. Further increase in concentration of p-Np caused decline in the value of k_app. Kinetic data reveals that catalytic reduction of p-Np obeys Langmuir–Hinshelwood mechanism and p-Np is converted to p-Ap on the surface of the silver nanoparticles passing through various reaction intermediates.     

Preparation and characterization of poly(ethylene carbonate)/poly(lactic acid) blends

Poly(ethylene carbonate)/poly(lactic acid) blends were successfully prepared by means of a solution film-casting method, and their physicochemical properties were investigated. PEC/PLA blends exhibit partial miscibility and are characterized by the interaction of the ester and carbonic ester groups. One such interaction is between partial charges in –C–O– in –O–C=O of PLA and the carbonyl –C=O of PEC. Another is between –C–O– in –O–C=O of PLA and –C–O– in –CH₂–O– of PEC. The value of T_g varies by more than 10 °C across the blends. PEC does not significantly influence the melting temperature of neat PLA, but non-spherical spherulites are formed in PEC-rich blends, whereas the spherulites are spherical with an average size of 30 μm in PLA-rich blends. Crystallization of PLA is influenced by the addition of flexible PEC and by the proportion of PLA in the blends. Interestingly, addition of at least 10 wt% PLA increased T_g, with a crystallinity, X_c of 47% and better thermal degradation properties, with the temperature at 5 wt% weight loss (T_d5) more than 30 °C higher than for neat PEC.     

Enzyme-Assisted Aqueous Extraction of Kalahari Melon Seed Oil: Optimization Using Response Surface Methodology

Enzymatic extraction of oil from Kalahari melon seeds was investigated and evaluated by response surface methodology (RSM). Two commercial protease enzyme products were used separately: Neutrase^® 0.8 L and Flavourzyme^® 1000 L from Novozymes (Bagsvaerd, Denmark). RSM was applied to model and optimize the reaction conditions namely concentration of enzyme (20–50 g kg^?1 of seed mass), initial pH of mixture (pH 5–9), incubation temperature (40–60 °C), and incubation time (12–36 h). Well fitting models were successfully established for both enzymes: Neutrase 0.8 L (R ² = 0.9410) and Flavourzyme 1000 L (R ² = 0.9574) through multiple linear regressions with backward elimination. Incubation time was the most significant reaction factor on oil yield for both enzymes. The optimal conditions for Neutrase 0.8 L were: an enzyme concentration of 25 g kg^?1, an initial pH of 7, a temperature at 58 °C and an incubation time of 31 h with constant shaking at 100 rpm. Centrifuging the mixture at 8,000g for 20 min separated the oil with a recovery of 68.58 ± 3.39%. The optimal conditions for Flavourzyme 1000 L were enzyme concentration of 21 g kg^?1, initial pH of 6, temperature at 50 °C and incubation time of 36 h. These optimum conditions yielded a 71.55 ± 1.28% oil recovery.     

Development of natural and synthetic polymer-based semi-interpenetrating polymer network for controlled drug delivery: optimization and in vitro evaluation studies

This research paper describes the development, optimization and in vitro characterization of chemically cross-linked pectin–polyvinyl alcohol-co-poly(2-Acrylamido-2-methylpropane sulfonic acid) semi-interpenetrating polymer network hydrogel [pectin–PVA-co-poly(AMPS) semi-IPN hydrogel] for controlled delivery of model drug tramadol HCl. Response surface methodology based on 3² factorial design was used for optimization and investigating the effect of independent factors: polymer-blend ratio (pectin:PVA = X ₁) and monomer (AMPS = X ₂) concentration on the dependent variables, swelling ratio (q _18th), percent drug release (R _18th, %), time required for 80 % drug release (t _{80 %}, h), drug encapsulation efficiency (DEE, %) and drug loaded contents (DLC, mg/g) in pectin-PVA-co-poly(AMPS) gels prepared by free radical polymerization. The optimized semi-IPN gel (FPP-10) showed controlled in vitro drug release (R _18th) of 56.34 % in 18 h, t _{80 %} of 30 h, and DEE of 23.40 %. These semi-IPN hydrogels were also characterized through SEM, FTIR, sol–gel analysis, swelling studies and drug release characteristics. Therefore, this newly synthesized polymeric network could be a potential polymeric system for controlled drug delivery of tramadol HCl for prolonged drug release.