Application of Poly (Agar-Co-Glycerol-Co-Sweet Almond Oil) Based Organo-Hydrogels as a Drug Delivery Material

In this study, it was aimed to investigate the synthesis, characterization and drug release behaviors of organo-hydrogels containing pH-sensitive Agar (A), Glycerol (G), Sweet Almond oil (Wu et al. in J Mol Struct 882:107–115, 2008). Organo-hydrogels, which contained Agar, Glycerol and different amounts of Sweet Almond oil, were synthesized via the free-radical polymerization reaction with emulsion technique using glutaraldehyde or methylene bis acrylamide crosslinkers. Then, the degree of swelling, bond structures, blood compatibility and antioxidant properties of the synthesized organo-hydrogels were examined. In addition, Organo-hydrogels which loaded with Ceftriaxone and Oxaliplatin were synthesized with the same polymerization reaction and release kinetics were investigated. In vitro release studies were performed at media similar pH to gastric fluid (pH 2.0), skin surface (pH 5.5), blood fluid (pH 7.4) and intestinal fluid (pH 8.0), at 37 °C. The effects on release of crosslinker type and sweet almond oil amount were investigated. Kinetic parameters were determined using release results and these results were applied to zero and first-order equations and Korsmeyer-Peppas and Higuchi equations. Diffusion exponential was calculated for drug diffusion of organo-hydrogels and values consistent with release results were found.

     

Biodegradable Microspheres for Controlled Release of an Antibiotic Ciprofloxacin

Ciprofloxacin (CF) loaded biodegradable microspheres of Poly(lactide-co-caprolactone)-PF127 (a poloxamer block copolymer of Ethylene Oxide/Propylene Oxide) were prepared by using solvent evaporation technique. The microspheres were characterized by differential scanning calorimetry (DSC) and X-ray diffractometry (X-RD) technique to confirm the polymorphism of ciproflaxacin (CF) drug. The X-RD and DSC techniques indicated molecular level dispersion of CF in the microspheres. Scanning electron micrographic images (SEM) of the microspheres indicated smooth surfaces of the spherical microspheres. Cumulative release characteristics of the matrices for CF, the antibiotic drug, were investigated in pH 7.4 media. It was possible to release CF in controlled manner up to 72 h. The developed ciprofloxacin loaded Poly(lactide-co-caprolactone)-PF127 microspheres were evaluated for preliminary antibacterial applications.     

Poly(Lactic Acid)-co-Aspartic Acid Copolymers: Possible Utilization in Drug Delivery Systems

The synthesis and characterization of poly(lactic acid)-co-aspartic acid copolymers (PLA-co-Asp) were presented. Subsequently, the synthesized PLA-co-Asp copolymers were tested as biodegradable carriers in drug delivery systems. PLA-co-Asp copolymers were synthesized by solution polycondensation procedure, using different molar ratios PLA/l-aspartic acid (2.33/1, 1/1, 1/2.33), manganese acetate and phosphoric acid as catalysts and N,N′-dimethyl formamide (DMF)/toluene as solvent mixture. The copolymers were characterized by FT-IR and ¹H-NMR spectroscopy, gel permeation chromatography (GPC), DSC and TG-DTG analyses. Diclofenac sodium, a non steroidal anti-inflammatory drug was subsequently loaded into PLA-co-Asp copolymers. The in vitro drug release experiments were done by dialysis of the copolymer/drug systems, in phosphate buffer solution (pH = 7.4, at 37 °C) and monitored by UV spectroscopy.     

Synthesis and Properties Modified Feather Keratin-Based Motor Oil Sorbing Cryogels with High Oil Holding Capacity

Oleic acid was used to modify keratin extracted from chicken feathers by free radical initiated graft copolymerization. Thereafter, the modified keratin was used for the synthesis of cryogels. The influence of oleic acid modification, the crosslinker content, and the protein concentration on the properties of the cryogels were investigated by Fourier transform infrared spectroscopy, scanning electron microscopy, SDS-PAGE, and through oil holding capacity tests. To enhance the sorption properties, the cryogels were crosslinked with glutaraldehyde. Varying protein concentration from 1.27 to 5.09 wt% and glutaraldehyde concentration from 0 to 5 wt% produced cryogels with oil holding capacity ranging from 4.56 to 10.76 g/g. The highest results exceeded the sorption capacity of previously published oleic acid modified woodchips (6.3 g/g) as well as polypropylene (6 g/g), which is the standard material used in industry.     

A Novel Hybrid 2,4-Dichlorophenoxy Acetate Bead from Modified Cassava Starch and Sodium Alginate with Modified Natural Rubber Coating

A novel herbicide bead was developed by phase separation, utilizing modified cassava starch (CSt), sodium alginate (SA) and 2,4-dichlorophenoxy acetate (2,4 DA), and the beads were also coated with natural rubber grafted with cassava starch (NR-graft-CSt) to aid their water resistance. The alginate gel beads with 65% entrapped 2,4 DA showed 90% release within 24 h. The incorporation of CSt in the beads markedly improved their encapsulation efficiency to 98% and sustained the release of the herbicide for 700 h. The water resistance was improved by coating the beads with NR-graft-CSt when compared with the pure CSt/SA bead. The synthesized bead has excellent potential for agricultural applications.     

Formulation and Characterization of Sodium Alginate g-Hydroxy Ethylacrylate Bio-Degradable Polymeric Beads: In Vitro Release Studies

Novel type of highly swollen beads were prepared by grafting 2-hydroxyethylacrylate onto biodegradable Sodium alginate (SA) via free-radical polymerization using potassium persulphate as an initiator and Triprolidine hydrochloride as a model drug. Evidence of grafting was obtained by fourier transform infrared spectroscopic technique. Morphological properties of the beads were studied by SEM analysis. Thermal properties and crystallinity of the beads were characterized using differential scanning calorimetry and thermogravimetric analysis and X-ray diffraction techniques, respectively. Dissolution experiments were performed to study the release profiles at 37?°C in phosphate buffer solution (pH-7.4). Effect of monomer content, crosslinking agent and drug/polymer ratio on swelling properties and release profiles were also comparatively studied. A dissolution result concludes that drug release decreases with increasing crosslinker content. The highest release (96%) was obtained for the beads prepared with 0.5?mL crosslinking agent. Equilibrium swelling degree also supports the drug release profiles confirming SA-g-HEA beads showed better release profiles compare to plain SA beads.     

Fabrication of Biodegradable Superabsorbent Using RSM Design for Controlled Release of KNO<Subscript>3</Subscript>

Present study envisaged the sequential experimental design approach for the development of biodegradable Gelatin-Tapoica/polyacrylamide superabsorbent. Percentage water uptake efficacy of candidate sample was optimized using Response Surface Methodology (RSM) design under microwave irradiation. Different process variables such as potassium persulphate and ammonium persulphate (KPS:APS) ratio, pH, reaction time concentration of acrylamide and N,N-methylene-bis-acrylamide (MBA) were investigated as a function of percentage swelling using sequential experimental design. Maximum liquid efficacy of 1550% was obtained at KPS:APS?=?1.0:0.5; acrylamide?=?7.67?×?10^?1 mol L^?1; MBA?=?1.76?×?10^?2 mol L^?1; pH 10 and time?=?110 s. The 3D crosslinked network formed was characterized using Fourier Transformation Infrared spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopic (SEM) techniques and thermal stability was ensured by Thermal gravimetric Analysis/Differential Thermal Analysis/Differential Thermal Gravimetric (TGA/DTA/DTG) studies. Superabsorbent synthesized could increase the moisture content in different type of soils and was found to enhance the water-holding capability of the soil upto 60 days in clayey, 40 days in sandy and 51 days in mixture of two soils under controlled conditions. Further, candidate polymer was investigated for the in-vitro controlled release of the KNO₃ with diffusion exponent ‘n’ was found to be 0.4326 indicating Fickian type diffusion. Also, initial diffusion coefficient (D_I?=?3.49?×?10^?5 m² h^?1) was found to be greater than the lateral diffusion coefficient (D_L?=?3.76?×?10^?6 m² h^?1) indicated rapid release of KNO₃ during initial hours with slow release afterwards. The ecofriendly nature of the synthesized polymer was also tested by conducting biodegradation studies and it was found to degrade upto 94% and 88.1% within 70 days with degradation rate of 1.34 and 1.26% per day using composting method and vermicomposting method respectively. So, the synthesized candidate polymer was found to be boon for agriculture-horticulture sector with wide applicability.     

Formulation and Evaluation of Matrix Type Transdermal Patch Containing Silver Nanoparticles

This research aimed to prepare the silver nanoparticles (AgNPs)-loaded antimicrobial wound dressing patch using ethyl cellulose as a matrix membrane and diethyl phthalate as a plasticizer. The polymer suspension was homogeneously mixed with plasticizer, and then added to the colloidal AgNPs suspension. This mixture was poured into Petri dish and subsequently dried in a hot air oven at 80?±?2 °C for 10 h. The minimum inhibition concentration of the colloidal AgNPs suspension was 2.5 µg/ml. The AgNPs-loaded antimicrobial wound dressing patch was evaluated for physical properties by differential scanning calorimeter, X-ray diffraction, scanning electron microscope, and in vitro study. The antimicrobial wound dressing patch did not exhibit any interaction between the matrix membrane and AgNPs. The AgNPs were evenly dispersed in the patch. The patch could control the release of silver at 102.98?±?4.11% over 12 h. Although the AgNPs-loaded antimicrobial wound dressing patches can be easily prepared by the simple method, in future studies antimicrobial wound dressing patch will be developed by employing different types of film forming agents.     

Effect of Poly(Vinyl Acetate) on Mechanical Properties and Characteristics of Poly(Lactic Acid)/Natural Rubber Blends

Natural rubber grafted with poly(vinyl acetate) copolymer (NR-g-PVAc) was synthesized by emulsion polymerization. Three graft copolymers were prepared with different PVAc contents: 1 % (G1), 5 % (G5) and 12 % (G12). Poly(lactic acid) (PLA) was melt blended with natural rubber (NR) and/or NR-g-PVAc in a twin screw extruder. The blends contained 10–20 wt% rubber. The notched Izod impact strength and tensile properties were determined from the compression molded specimens. The effect of NR mastication on the mechanical properties of the PLA/NR/NR-g-PVAc blend was evaluated. Characterization by DMTA and DSC showed an enhancement in miscibility of the PLA/NR-g-PVAc blend. The temperature of the maximum tan δ of the PLA decreased with increasing PVAc content in the graft copolymer, i.e., from 71 °C (pure PLA) to 63 °C (the blend containing 10 % G12). The increase in miscibility brought about a reduction in the rubber particle diameter. These changes were attributed to the enhancement of toughness and ductility of PLA after blending with NR-g-PVAc. Therefore, NR-g-PVAc could be used as a toughening agent of PLA and as a compatibilizer of the PLA/NR blend. NR mastication was an efficient method for increasing the toughness and ductility of the blends which depended on the blend composition and the number of mastications.     

Biodegradation Study of Starch-graft-Acrylonitrile Copolymer

In this study the biodegradability of starch-graft-acrylonitrile (St-g-AN) copolymer has been investigated using some microorganisms including Aspergillus niger. The fungus A. niger was isolated from the soil and from the wastewater of an acrylic fiber company. The effects of four factors including environment temperature, primary inoculum concentration, pH and weight of copolymer film, on the biomass generation as a measure of biodegradation rate of copolymer, were studied using Taguchi experimental design. The statistical analysis of the results showed that the primary inoculum concentration and temperature were the most important factors affecting the biodegradation of St-g-AN copolymer. The optimum levels of temperature, pH, inoculum concentration, and weight of films to attain the maximum biodegradation (as much as 8.59 % by weight percentage during 28 days) were obtained as 30 °C, 4.75, 10⁸ spore/mL, and 1.1 g, respectively. The changes in the structure and morphological properties of the copolymer before and after degradation were determined using transform infrared spectroscopy and scanning electron microscopy.     

Optimized Removal of Acid Blue 62 from Textile Waste Water by SBA-15/PAMAM Dendrimer Hybrid Using Response Surface Methodology

SBA-15/PAMAM Nano adsorbent was synthesized by the proficiency of SBA-15 as an original compound, 3-chloropropyltrimethoxysilane as a bridge chemical compound and polyamidoamine dendrimer (PAMAM) in the role of a multifunctional amine end group for adsorption of acid blue 62 (AB62) from aqueous media. The synthesized adsorbent was characterized by transmission electron microscope, field emission scanning electron microscope and Fourier-transform infrared spectroscope. A response surface methodology was employed to evaluate the simple and amalgamated factors of the operating variables subtending initial pH (2–12), adsorbent dosage(0.01–0.03 g), contact time (5–120 min), initial dye concentration (40–600 ppm) and temperature (25–45?°C) to optimize the operating statues of the treatment method. These parameters were altered at five levels pursuant to the central composite design to appraise their effects on AB62 removal through analysis of variance. Analysis of variance represented a high coefficient of definition amount (R²?=?0.9999) and acceptable prediction quadratic polynomial model was concluded which ascertain the suitability of the model and a high correlation among the predicted and empirical amounts. Utmost color removal efficiency was auspicated and empirically accredited. The optimum conditions relied on acquired results for AB62 removal were at an initial pH of 2, adsorbent dosage of 0.03 g SBA-15/PAMAM, dye concentration of 40 mg l^?1, time contact of 60 min and temperature of 25?°C.     

Novel Bioactive Chiral Poly(amide–imide)s Containing Different Amino Acids Linkages: Studies on Synthesis, Characterization and Biodegradability

In this paper chiral bioactive poly(amide–imide)s (PAI)s were synthesized from four different diacids containing chiral amino acids with 4,4′-methylene bis(3-chloro 2,6-diethylaniline) as a diamine via direct polycondensation reaction in a system of tetra-n-butylammonium bromide and triphenyl phosphite as a condensing agent. The structures of these polymers were confirmed by FT-IR, ¹H-NMR, specific rotation, elemental and thermogravimetric analysis (TGA) techniques. TGA showed that the 10 % weight loss temperature in a nitrogen atmosphere was more than 378 °C, which indicates that the resulting PAIs have a good thermal stability. The biodegradability of the monomers and prepared polymers was investigated in culture media and soil burial test for assessment of the susceptibility of these compounds to microbial degradation. The results showed that the synthesized monomers and theirs derived polymers are biologically active and nontoxic to microbial growth.     

A Biobased Blend of Cellulose Diacetate with Starch

Two bio-based polymers, cellulose diacetate (CDA) and starch, were used to prepare blends with reasonable properties and low cost. Due to the poor processing properties, starch was modified in the presence of glycerol and epoxidized soybean oil (ESO), and CDA was plasticized by triacetin (TA) and ESO, respectively. The morphologies of the blends with different amounts of modified starch (MST) were studied by scanning electron microscope (SEM), and the physical properties of the blends, including thermal stability, mechanical property, water and moisture resistance, were investigated. The equilibrium moisture absorption rates of the blends containing 30 and 50 wt% MST at 100 % of relative humidity(RH) were 9.4 and 15.0 %, respectively. SEM and DMA results demonstrated that CDA and MST had a certain extent of compatibility. Due to the partial plasticization of starch, the tensile strength of the blends was nearly not affected by the amount of MST. Even if 50 wt% MST was added, the tensile strength of the blend was as high as 24.7 MPa. The obtained blend containing 30 wt% MST can keep good mechanical properties at 50 % RH, and its tensile strength and elongation at break are 30.2 MPa and 3.6 %, respectively. All the results show that the CDA/MST blends have a potential as an environmental friendly material.     

Recycling of the hyperaccumulator Brassica juncea L.: synthesis of carbon nanotube-Cu/ZnO nanocomposites

The methods of synthesizing carbon nanotube (CNTs)-Cu/ZnO nanocomposites using a Cu hyperaccumulator (Brassica juncea L.) constitute a new insight into the recycling of hyperaccumulators and provide a new route for the further development of green nanostructure syntheses. In this paper, CNTs-Cu/ZnO nanocomposites have been synthesized using B. juncea plants as the sources of C, Cu, and Zn. The synthesized CNTs-Cu/ZnO nanocomposites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectra (EDS). The synthesized CNTs were characterized further by selected area diffraction (SAD) patterns and Raman spectroscopy. The results demonstrated that the structure of individual CNTs was middle-hollow, with an outer diameter of about 80 nm. The synthesized CNTs were not at all crystalline and there were a few defects in the walls. The outer diameter of CNTs-Cu/ZnO nanocomposites was 110 nm. The diameters of Cu/ZnO nanoparticles were 29.5/32.7 nm, respectively. Cu/ZnO nanoparticles that had grown onto the CNT surface were nonuniform and agglomerated. The Cu/ZnO nanoparticles were pure.     

Treatment of discarded oil in supercritical carbon dioxide for preparation of carbon microspheres

Carbon microspheres with diameter of 1–10 μm were prepared by treatment of waste oil in a supercritical carbon dioxide (scCO₂) system. The structure and morphology of the products were characterized by X-ray diffraction, field-emission scanning electron microscopy, and Raman spectrometry. It is shown that the products consist of graphite microspheres with relatively low graphitization. The yield of solid products increased from 26.8 wt% to 42.2 wt% as the reaction temperature was raised from 530°C to 600°C. Spheres with multilayer structure could be obtained by means of subsequent vacuum annealing of the carbon microspheres at 1500°C. The formation mechanisms of carbon microspheres in the scCO₂ system and the influence of vacuum annealing on the structure are discussed in detail.     

Characterization of Atrazine-Loaded Biodegradable Poly(Hydroxybutyrate-Co-Hydroxyvalerate) Microspheres

Polyhydroxybutyrate-co-hydroxyvalerate microspheres (PHBV-MS) were prepared as a delivery system for the herbicide atrazine (ATZ). Characterization of the system included investigation of in vitro release properties and genotoxicity. ATZ − PHBV-MS particle diameters showed a size distribution range of 1–13 μm. Differential scanning calorimetry analyses indicated that ATZ was associated with the PHBV microparticles. The release profiles showed a different release behavior for the pure herbicide in solution, as compared with that containing ATZ-loaded PHBV-MS. Korsmeyer–Peppas model analyses showed that atrazine release from the microparticles occurred by a combination of diffusion through the matrix and partial diffusion through water-filled pores of the PHBV microparticles. A Lactuca sativa test result showed that the genotoxicity of ATZ-loaded PHBV-MP was decreased in relation to ATZ alone. The results demonstrate a viable biodegradable herbicide release system using atrazine for agrochemical purposes.     

Production of Poly(3-hydroxyalkanoate)s by Pseudomonas putida Cultivated in a Glycerol/Nonanoic Acid-Containing Medium

The biosynthesis of poly(3-hydroxyalkanoate) (PHA) by Pseudomonas putida (JCM6160) cultivated in a medium containing glycerol, nonanoic acid, or a glycerol/nonanoic acid mixture as the sole carbon sources was investigated. The PHA content was ~20 % when glycerol was the carbon source. This relatively low content can be attributed to the glycerol end-cap effect and the absence of enzymes that can directly synthesize PHA from acetyl CoA, which is the major metabolite of glycerol. Fatty acids, containing even numbered carbons, are synthesized from acetyl CoA, and they can be used as substrates for PHA synthesis. However, this process also results in decreasing PHA content as fatty acids are siphoned off into other pathways. However, addition of 5 mM nonanoic acid into a 20 mM glycerol-containing medium dramatically increased the PHA content in P. putida, which was 1.3 times larger than the sum of the values found when glycerol and nonanoic acid were each used as the sole carbon source. The PHA, synthesized in the glycerol/nonanoic acid medium, contains 3-hydroxy alkanoate units that have 5, 6, 7, 8, 9, or 10 carbons. The units that contain the even numbered carbons are derived from fatty acids that were produced from glycerol; whereas, the PHA units with the odd numbered carbons are derived from nonanoic acid. Pentanoate units were also found in the polyester derived from glycerol and nonanoic acid, and must have been synthesized indirectly via β-oxidation of nonanoic acid with the assistance of glycerol because pentanoate units were not found in PHA when P. putida was cultivated in the presence of only nonanoic acid.     

Immobilization of copper ions laden kaolin waste: influence of thermal treatment on its immobilization in cement paste

This work aims to study the influence of thermal treatment of Cu²⁺ laden kaolin wastes on its immobilization efficiency in cement paste. Compressive strength and toxicity characteristic leaching procedure (TCLP) of 5–20 % kaolin waste blended cement pastes were tested. X-ray diffraction (XRD) results illustrate that adsorption of Cu²⁺ ions modify the crystal structure of kaolinite mineral. Fourier transform infrared (FTIR) results indicate that the adsorption sites on the kaolin surface that were occupied with free water molecules have been replaced with Cu²⁺ ions adsorbed from aqueous solutions. The thermal treatment of kaolin waste improves fixation ratio of Cu²⁺ in cement pastes containing up to 20 % of thermally treated waste. This is due to: pozzolanic activity of calcined kaolin, conversion of leachable adsorbed Cu²⁺ ions into encapsulated unleachable phase that does not retard the hydration of cement as well as adsorption of much of leachable Cu²⁺ ions on surfaces of hydration products and occlusion in its lattice structure as illustrated from XRD, FTIR, thermogravimetric, scanning electron microscopy and TCLP results. The fixation ratio of Cu²⁺ in cement paste blended with 20 % of thermally treated kaolin waste, reaches maximum value of about 97 % compared to 82 % for cement paste blended with 20 % of untreated kaolin waste.     

Potassium Release Kinetics and Water Retention of Controlled-Release Fertilizers Based on Chitosan Hydrogels

Controlled release fertilizer (CRF) hydrogels were prepared from poly(vinyl alcohol), poly(vinyl alcohol)/chitosan and chitosan using glutaraldehyde as a crosslinker. Intermolecular interactions of the CRF hydrogels were elucidated using FTIR. Water absorbency characteristics of the CRF hydrogels were also studied. It was found that the CRF hydrogels exhibited the equilibrium swelling ratio (SR) in the range 70–300%. The water retention of soil containing the CRF hydrogels was also examined. It was found that the CRF hydrogels increased the water retention of the soil. After 30 days, soil containing the PVA-, PVA/CS- and CS-hydrogels showed the water retention capacities of 25%, 10% and 4%, respectively. While the soil without the CRF hydrogel had already given off most of the water. The release behavior of potassium from the CRF hydrogels, both in deionized water and in soil, was investigated. In soil, the potassium release mechanism from the PVA- and PVA/CS-hydrogels were non-Fickian diffusion. On the other hand, the CS hydrogel showed, n value that was close to 1.0 corresponding to case II transport. In deionized water, all the CRF hydrogels showed small values of release exponent (n < 0.5) indicating a quasi-Fickian diffusion mechanism.     

Crosslinked Poly(2-Hydroxyethyl Methacrylate) by Emulsion Templating: Influence of Crosslinker on Microcellular Structure

The synthesis of microcellular porous polymers based on 2-hydroxyethyl methacrylate (HEMA) by free radical polymerisation of a continuous phase of high internal phase emulsion (HIPE) is reported. N,N’-methylene bisacrylamide (MBAA) and glutaraldehyde are used as crosslinking agents. GA is added to the monomer phase either during the emulsion preparation or post polymerisation crosslinking of HEMA is performed. The crosslinker influences the morphological structure of porous poly(HEMA) materials. In the case of using MBAA as the crosslinker, homogeneous polyHIPE structure is obtained, with average cavities diameter approximately 8 μm and interconnecting pore diameter approximately 3 μm. In the case of using GA in situ crosslinking a polyHIPE is obtained exhibiting cavities of diameter approximately 12 μm and interconnecting pores of approximately 3 μm. Post polymerisation crosslinking with GA influence the structural features resulting in a different morphology. Samples are characterised using FTIR spectroscopy, scanning electron microscopy, nitrogen adsorption and swelling behaviour measurements. Polymers are prepared in the form of monoliths and membranes.