Bioassay and bioactivity of polymer as carrier for some active compounds such as anticancer drugs

The present work deals with the development of a new slow release polymeric material, based on maize starch/cellulose acetate blend polymerized with acrylic acid monomer by free-radical mechanism. The polymerization was initiated by a redox system. The synthesized polymeric material may be used as a carrier for some active compounds such as anticancer drugs and has been characterized by Fourier transform spectroscopy. The active compounds are a new series of heterocyclic derivatives that had an anticancer effect and were prepared from pyrimidine and coumarin compounds, namely: 7-(2-methoxyphenyl)-5-thioxo-5,6-dihydro[1,2,4]triazolo[4,3-c] pyrimidine-8-carbonitrile (compound I), 8-(2-methoxyphenyl)-3,4-dioxo-6-thioxo-3,4,6,7-tetrahydro-2h-pyrimido[6,1-c]-[1,2,4]triazine-9-carbonitrile (compound II), and 4-substituted-1-(1-(7-methoxy-4-methyl-coumarin-8-yl) ethylidene) thiosemi-carbazide (compound III). They were incorporated into the prepared polymer matrix. The polymer-carried drug was tested for slow release drug delivery through testing it in aqueous media for different time periods and examining it as an anti-proliferative agent against human liver cancer cell line (HEPG2). The release rate of the drug was evaluated in aqueous media at different pHs as well as in dimethyl formamide which is the good solvent of such drugs. The release was measured spectrophotometrically. It was found that the release rate depends on the pH of the aqueous media. The release of the drug in the alkaline media was found to be high compared with other media. Also, the sustained release of the drug was extended to about 20 days. The activity of the released drug against human liver cancer cell line was tested. The results showed that compound (III) gave the highest growth inhibition activity followed by compound (II), while compound (I) indicated the lowest activity against the human liver (HEPG2) cancer cell line.     

Proton-conducting membranes: poly (N-vinyl pyrrolidone) complexes with various ammonium salts

The present study focuses on the proton-conducting polymer electrolytes; poly (N-vinyl pyrrolidone)–ammonium thiocyanate and poly (N-vinyl pyrrolidone)–ammonium acetate prepared by solution casting technique. The XRD analysis indicates the amorphous nature of the polymer electrolytes. The Raman spectra of the C=O vibration of pure polymer PVP at 1,663 cm^?1 has been appeared as doublet in the polymer electrolytes. The introduction of this new peak in the salt-doped polymer electrolytes may be due to interaction of the cation with the polymer. The room temperature ionic conductivity σ _303κ has been found to be high, 1.7?×?10^?4 S cm^?1 for 80 mol% PVP–20 mol% NH₄SCN and 1.5?×?10^?6 S cm^?1 for 75 mol% PVP–25 mol% CH₃COONH₄. The polymer electrolytes have been tested for their application in Zn–air battery.     

Enhancing the Cellulose-Degrading Activity of Cellulolytic Bacteria CTL-6 (Clostridium thermocellum) by Co-Culture with Non-cellulolytic Bacteria W2-10 (Geobacillus sp.)

The effect of a non-cellulolytic bacterium W2-10 (Geobacillus sp.) on the cellulose-degrading activity of a cellulolytic bacterium CTL-6 (Clostridium thermocellum) was determined using cellulose materials (paper and straw) in peptone cellulose solution (PCS) medium under aerobic conditions. The results indicated that in the co-culture, addition of W2-10 resulted in a balanced medium pH, and may provide the required anaerobic environment for CTL-6. Overall, addition of W2-10 was beneficial to CTL-6 growth in the adverse environment of the PCS medium. In co-culture with W2-10, the CTL-6 cellulose degradation efficiency of filter paper and alkaline-treated wheat straw significantly increased up to 72.45 and 37.79 %, respectively. The CMCase activity and biomass of CTL-6 also increased from 0.23 U ml^?1 and 45.1 μg ml^?1 (DNA content) up to 0.47 U ml^?1 and 112.2 μg ml^?1, respectively. In addition, co-culture resulted in accumulation of acetate and propionate up to 4.26 and 2.76 mg ml^?1. This was a respective increase of 2.58 and 4.45 times, in comparison to the monoculture with CTL-6.     

Fabrication,characterization and evaluation of bacterial cellulose-based capsule shells for oral drug delivery

Bacterial cellulose (BC) was investigated for the first time for the preparation of capsule shells for immediate and sustained release of drugs. The prepared capsule shells were characterized using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The BC capsule shells were studied for drug release using an USP type-I dissolution apparatus. Irrespective of the drying method and the thickness of the BC sheet, the capsule shells displayed an immediate drug release profile. Moreover, the addition of release-retardant cellulosic polymers sustained the drug release having first-order kinetics for hydroxypropylmethylcellulose and carboxymethyl cellulose sodium with R ² values of 0.9995 and 0.9954, respectively. Furthermore, these capsules shells remained buoyant in 0.1 N HCl (pH 1.2) solution up to 12 h. This study showed that BC is a promising alternative to gelatin capsules with both immediate and sustained drug release properties depending upon the compositions of the encapsulated materials.     

Conductivity and Dielectric Behavior Studies of Carboxymethyl Cellulose from Kenaf Bast Fiber Incorporated with Ammonium Acetate-BMATFSI Biopolymer Electrolytes

This work was undertaken to study the conductivity and dielectric behavior of a biopolymer electrolyte based on carboxymethyl cellulose that was synthesized from kenaf fiber. Biopolymer electrolytes comprised of various weight percentage ratios of the host polymer, ammonium acetate salt, and butyl-trimethyl ammonium bis(trifluoromethylsulfonyl)imide ionic liquid were prepared by the solution casting technique. The conductivity values were determined by impedance spectroscopy. The highest conductivity found was 2.18 × 10^?3 S cm^?1 at ambient temperature for the film incorporated with 20 wt.% salt and 20 wt.% ionic liquid. In order to understand the conductivity behavior, a dielectric study was carried out. The results showed that the system obeys the Arrhenius rule and confirmed non-Debye behavior in the sample.     

Cyproterone Synthesis, Recognition and Controlled Release by Molecularly Imprinted Nanoparticle

In this study, we used novel synthetic conditions of precipitation polymerization to obtain nanosized cyproterone molecularly imprinted polymers for application in the design of new drug delivery systems. The scanning electron microscopy images and Brunauer?CEmmett?CTeller analysis showed that molecularly imprinted polymer (MIP) prepared by acetonitrile exhibited particles at the nanoscale with a high degree of monodispersity, specific surface area of 246?m²?g^?1, and pore volume of 1.24?cm³?g^?1. In addition, drug release, binding properties, and dynamic light scattering of molecularly imprinted polymers were studied. Selectivity of MIPs was evaluated by comparing several substances with similar molecular structures to that of cyproterone. Controlled release of cyproterone from nanoparticles was investigated through in vitro dissolution tests and by measuring the absorbance by HPLC-UV. The pH dissolution media employed in controlled release studies were 1.0 at 37?°C for 5?h and then at pH 6.8 using the pH change method. Results show that MIPs have a better ability to control the cyproterone release in a physiological medium compared to the non molecularly imprinted polymers (NMIPs).     

A Validated LC Method for the Quantitation of Cefotaxime in pH-Sensitive Nanoparticles

A sensitive and rapid routine LC method was validated for measuring cefotaxime incorporated in three different pH-sensitive nanoparticles. The drug was chromatographed on a C18 reversed-phase column; the mobile phase used was 0.05 M aqueous ammonium acetate, acetonitrile and tetrahydrofuran (87:11:2, v/v) adjusted to pH 5.5 with acetic acid. The flow rate was 1 mL min^?1 and cefotaxime was quantified at 254 nm, with a sensitivity range of 0.005 AUFS. The validated method was specific, linear (R ² ≥ 0.999), precise and accurate in a concentration range of 0.2–50.0 μg mL^?1. The method was rapid, selective and suitable for evaluation of cefotaxime in pH-sensitive Eudragit nanoparticles.     

Development of an enantioselective membrane from cellulose acetate propionate/cellulose acetate,for the separation of trans-stilbene oxide

This paper reports the characterization of new synthesized chiral polymeric membranes, based on a cellulose acetate propionate polymer. The flux and permselective properties of the membrane were studied using 50 % ethanol solution of (R,S)-trans-stilbene oxide as feed solution. Scanning electron microscopy revealed the asymmetric structure of these membranes. The roughness of the surface was measured by atomic force microscopy. The resolution of over 97 % enantiomeric excess was achieved when the enantioselective membrane was prepared with 18 wt% cellulose acetate and 8 wt% cellulose acetate propionate in the casting solution of dimethyl formamide/N-methyl-2-pyrrolidone/acetone, at 20 °C and 55 % humidity, and a water bath at 10 °C for the gelation of the membrane. The operating pressure and the feed concentration of the trans-stilbene oxide were 275.57, 345.19, and 413.84 kPa and 2.6 mM, respectively.     

Electrospun cellulose acetate/poly(vinylidene fluoride) nanofibrous membrane for polymer lithium-ion batteries

The membranes for gel polymer electrolyte (GPE) for lithium-ion batteries were prepared by electrospinning a blend of poly(vinylidene fluoride) (PVdF) with cellulose acetate (CA). The performances of the prepared membranes and the resulted GPEs were investigated, including scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), X-ray diffraction (XRD), porosity, hydrophilicity, electrolyte uptake, mechanical property, thermal stability, AC impedance measurements, linear sweep voltammetry, and charge–discharge cycle tests. The effect of the ratio of CA to PVdF on the performance of the prepared membranes was considered. It is found that the GPE based on the blended polymer with CA:PVdF =2:8 (in weight) has an outstanding combination property-strength (11.1 MPa), electrolyte uptake (768.2 %), thermal stability (no shrinkage under 80 °C without tension), and ionic conductivity (2.61 × 10^?3 S cm^?1). The Li/GPE/LiCoO₂ battery using this GPE exhibits superior cyclic stability and storage performance at room temperature. Its specific capacity reaches up to 204.15 mAh g^?1, with embedded lithium capacity utilization rate of 74.94 %, which is higher than the other lithium-ion batteries with the same cathode material LiCoO₂ (about 50 %).     

Development and Validation of a Stability Indicating LC Method for the Determination of Faropenem in Pharmaceutical Formulations

A simple, selective and sensitive stability indicating LC method has been developed and validated for the determination of faropenem in bulk drug and pharmaceutical formulations in the presence of degradation products. The separation was achieved by using an isocratic mobile phase mixture of acetate buffer of pH 3.5 and methanol (65:35, v/v) and 250 mm × 4.6 mm I.D., 5 μm particle size SGE make Wakosil C-18 AR column at flow rate of 1.0 mL min^?1 with detection at 305 nm. The retention time of faropenem is 6.63 min and was linear in the range of 5–75 μg mL^?1 (r = 0.9999). The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation and was found to be unstable in all the stress conditions. The proposed method was successfully employed for quantification of faropenem in bulk drug and its pharmaceutical formulations.     

Synthesis and characterization of carboxymethyl cellulose-silver nanoparticle (AgNp)-silica hybrid for amylase immobilization

Carboxymethyl cellulose-silver nanoparticle (AgNp)-silica hybrids have been synthesized in a modified Stöber process. The hybrid synthesis was optimized to obtain an efficient immobilization matrix for diastase alpha amylase, a multimeric enzyme of high technological significance. The synthesized hybrids were characterized using FTIR, XRD, SEM, TGA and BET studies. The enzyme immobilization was done by adsorption and using the immobilized enzyme, the hydrolysis of soluble starch has been optimized in comparison to free enzyme. The optimum usable pH for the immobilized enzyme ranged from pH 4 to 5, while pH 5 was optimum pH for the free enzyme activity. The kinetic parameters for the immobilized, (K _M = 3.4610 mg ml^?1; V _max = 6.3540 mg ml^?1 min^?1) and free enzyme (K _M = 4.1664 mg ml^?1; V _max = 4.291 mg ml^?1 min^?1) hydrolysis indicated that the immobilization at the nanohybrid has significantly improved the catalytic property of the enzyme. In the immobilized state, the enzyme remained usable for many repeated cycles like our previous material, gum acacia-gelatin-AgNp-silica. Storage experiments indicated that the immobilization has increased the stability of the enzyme and also that AgNps play a role in stabilizing the immobilized enzyme.     

Employment of [Amim] Cl in the effort to upgrade the properties of cellulose acetate based polymer electrolytes

Transparent thin film polymer electrolytes were prepared by solvent casting technique with the doping of environmental-friendly ionic liquid, 1-allyl-3-methylimidazolium chloride ([Amim] Cl) into the matrix formed by cellulose acetate (CA) and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI). The ionic conducting nature of this system improves significantly from the order of 10^?7–10^?2 S cm^?1 upon increasing doping of [Amim] Cl content till a maximum of 4.68 × 10^?2 S cm^?1 is attained for the composition CA:LiTFSI:[Amim] Cl (14:6:80 wt%). The improving trend in ionic conductivity results from the bond weakening between the connecting atoms in the crystalline region that induces to the increase in amorphous counterpart fractions in the CA matrix. This observation was proved via the accountancies in the reduction of relative viscosity, root mean square value and increase in void as increase in [Amim] Cl doping. The resultant phase conversion hence permits immense lithium ion (Li⁺) fluidity along the polymer backbone and assisting the improvement in ionic conductivity. The thin film polymer electrolyte is found to be elastic in the presence of crystalline fraction and radically deforms upon the chains diffusion into the amorphous fraction. The linear curvatures of the Arrhenius plot justify the conductivity improvement as via the increasing frequency of Li⁺ ions hopping as the temperature increases. The increasing addition of [Amim] Cl diminishes both the heat-resistivity and thermal stability of CA:LiTFSI:[Amim] Cl matrix.     

Forced Degradation Study to Develop and Validate Stability-Indicating RP-LC for Quantification of Ropinirole Hydrochloride in Its Modified Release Tablets

A forced degradation study on ropinirole hydrochloride in bulk and in its modified release tablets was conducted under the conditions of hydrolysis, oxidation and photolysis in order to develop an isocratic stability-indicating LC-UV method for quantification of the drug in tablets. An impurity peak in standard solution was found to increase under acidic and neutral hydrolytic conditions while another degradation product was formed under alkaline condition. The drug and its degradation products were optimally resolved on a Hypersil C₁₈ column with mobile phase composed of diammonium hydrogen orthophosphate (0.05 M; pH 7.2), tetrahydrofuran and methanol (80:15:5% v/v) at a flow rate of 1.0 mL min^?1 at 30 °C using 250 nm as detection wavelength. The method was linear in the range of 0.05–50 μg mL^?1 drug concentrations. The %RSD of inter- and intra-day precision studies was <1. The system suitability parameters remained unaffected during quantification of the drug on three different LC systems. Excellent recoveries (101.59–102.28%) proved that the method was sufficiently accurate. The LOD and LOQ were found to be 0.012 and 0.040 μg mL^?1, respectively. Degradation behaviour of the drug in both bulk and tablets was similar. The drug was very unstable to hydrolytic conditions but stable to oxidative and photolytic conditions. The method can be used for rapid and accurate quantification of ropinirole hydrochloride in tablets during stability testing. Based on chemical reactivity of ropinirole in different media, the degradation products were suspected to be different from the known impurities of the drug.     

Treatment of chromium effluent by adsorption on chitosan activated with ionic liquids

This study proposes, verifies, and refines the use of biopolymers treated with two new ionic liquids (ILs) (sec-butylammonium acetate and n-octylammonium acetate), as a platform for chromium adsorption. The ILs were synthesized, characterized, and applied to chitosan treatment. Analyzing the size distribution of microparticles of chitosan and chitosan activated with ILs (sec-butylammonium acetate and n-octylammonium acetate), we observed that a little decrease in the particle size occurred with the activation of chitosan (176 ± 0.02 μm to 167 ± 0.054 and 168.5 ± 0.05 μm, respectively), as well as changes in the X-ray diffraction FTIR_ATR spectra. Further studies were performed using the best adsorbent – chitosan treated with sec-butylammonium acetate. In this case, the chromium VI concentration in the sample was reduced by more than 99% when using chitosan treated with IL sec-butylammonium acetate. The best reaction time was determined as 1 h, which allowed a chromium adsorption of 99.1% and the adsorption kinetic data were best represented by the second-order model (k₂ = 11.7258 g mg^?1 min^?1). The maximum adsorption capacity was obtained using the Langmuir isotherm model (20.833 mg g^?1 at pH 4 during 1 h, using 1.0 g of chitosan), and the adsorption efficiency was enhanced at 25 °C by the Freundlich isotherm model, in which the constants KF and n were determined as 0.875 mg L^?1 and 1.610, respectively.     

Synthesis of Carboxymethyl Cellulose Based Drug Carrier Hydrogel Using Ionizing Radiation for Possible Use as Site Specific Delivery System

A unique natural polymer based colon specific drug carrier was prepared from carboxymethyl cellulose (CMC) and acrylic acid (AAc) in aqueous solution employing γ‐radiation induced copolymerization and crosslinking. The effect of preparation conditions such as the natural polymer content and irradiation dose on gelation process was investigated. The swelling behavior of the prepared hydrogels was characterized by investigating the time and pH dependent swelling of the (CMC/AAc) hydrogels of different CMC content. The effects of the hydrogel composition and pH of the swelling medium on the swelling indices were estimated. The results show that the increment in the CMC content in the feed solution enhances the gelation process. The results also show the dependence of the swelling indices on both hydrogel composition and pH value of the swelling medium. To evaluate the ability of the prepared hydrogel to be used as a colon‐specific drug carrier, the release profile of theophylline was studied as a function of time at pH 1 and pH 7.     

Preparation and characterization of poly(styrene-alt-maleic acid)-b-polystyrene block copolymer self-assembled nanoparticles

Block copolymers poly(styrene-alt-maleic anhydride)-b-polystyrene (P(St-alt-MAn)-b-PSt) were synthesized via radical addition fragmentation chain transfer copolymerization. The maleic anhydride-containing segments of the block copolymer were hydrolyzed to form amphiphilic poly(styrene-alt-maleic acid)-b-polystyrene (P(St-alt-MA)-b-PSt). In aqueous solution, P(St-alt-MA)₇₃-b-PSt₈₁ and P(St-alt-MA)₅₈-b-PSt₁₃₀ formed stable dispersed spherical aggregates of approximately 25 and 40 nm, respectively. Particle size was stable under alkaline conditions and was little affected by the polymer concentration in the range of 0.025–1.0 mg mL^?1. The critical aggregation concentrations of the block copolymer self-aggregates were 1?×?10^?3 and 3?×?10^?3 mg mL^?1 for hydrophobic PSt block lengths of 130 and 81 monomer units, respectively. The nanoparticles had a negative surface charge at pH?>?2. Scanning electron microscopy images revealed that particle–particle coalescence did not occur upon drying of the film and the nanoparticles remained discrete. Controlled aspirin release from the nanoparticles was dependent on the structure of the block polymers and release medium.     

Adsorption of Hg(II) Ions onto Binary Biopolymeric Beads of Carboxymethyl Cellulose and Alginate

The removal of Hg(II) ions from aqueous solution by adsorption onto cross-linked polymeric beads of carboxymethyl cellulose (CMC) and sodium alginate was studied at fixed pH (6) and room temperature 28 ± 0.2°C. The cross-linked polymeric beads were characterized by FTIR spectra. Sorption capacity of the polymer for the mercury ions was investigated in aqueous media consisting different amounts of mercury ions (2.5 to 100 mg dm^?3) and at different pH values (2 to 8). Adsorption behavior of Hg(II) ions could be modeled using both the Langmuir and Freundlich isotherms. The dynamic nature of adsorption was quantified in terms of several kinetic constants such as rate constants for adsorption (k₁) and Lagergreen rate constant (K_ad). The influence of various experimental parameters such as effect of pH, contact time, solid-to-liquid ratio, salt effect, and temperature effect etc. were investigated on the adsorption of Hg(II) ions.     

Use of Mesophilic Fungal Amylases Produced by Solid-state Fermentation in the Cold Hydrolysis of Raw Babassu Cake Starch

Amylases constitute one of the most important groups of industrial enzymes, presenting several applications, such as in the food, textile, and ethanol manufacturing. In this work, a starchy residue from the Brazilian agroindustry, namely babassu cake, was used for the production of amylases by solid-state fermentation and for obtaining sugar hydrolysates, which can be used as building blocks for future bioconversions. Eight filamentous fungi from the genera Aspergillus and Penicillium were screened. Regarding amylase production, A. awamori strains showed well-balanced endoamylase and exoamylase activities, while A. wentii produced an amylolytic complex much richer in the endo-acting enzymes. Simultaneous liquefaction and saccharification using the crude enzyme extracts from the four most promising fungal strains was then investigated applying DOE techniques. The highest total reducing sugar content (24.70 g L^?1) was obtained by the crude extract from A. awamori IOC-3914, corresponding to a hydrolysis yield of 52% of total starch in the cake, while A. awamori IOC-3915 produced the most appropriate extract in terms of glucose release (maximum of 5.52 g L^?1). Multivariate analysis of the DOE studies indicated that these extracts showed their best performance at 50–57 °C under acid conditions (pH 3.6–4.5), but were also able to act satisfactorily under milder conditions (36 °C and pH 5.0), when TRS and glucose released were about 65% of the maximum values obtained. These data confirm the high potential of the enzyme extracts under study for cold hydrolysis of starch.     

Metabolic Profile of Nitazoxanide in Goat Feces

A sensitive and specific method for the identification of nitazoxanide metabolites in goat feces by liquid chromatography–electrospray ionization tandem mass spectrometry with negative ion mode was developed. After extraction procedure the pretreated samples were injected on an XTerra MS C8 column with mobile phase (0.2 mL min^?1) of acetonitrile and 10 mM ammonium acetate (adjusted to pH 2.5 with formic acid) followed by a linear gradient elution, and detected by MS–MS. Identification and structural elucidation of the metabolites were performed by comparing their retention times (R _t ), full scan, product ion scan, precursor ion scan and neutral loss scan MS–MS spectra to those of the parent drug or other available standard. The parent drug (nitazoxanide) and its deacetyl metabolite (tizoxanide) were found in goat feces after the administration of a single oral dose of 200 mg kg^?1 of nitazoxanide. Tizoxanide was detected in goat feces for up to 96 h after ingestion of nitazoxanide.     

Preparation and characterization of cellulose acetate complexes

Summary Metal chelates of secondary cellulose acetate (SCA) with chromium(III), copper(II), cobalt(II), nickel(II) and UO ₂ ²⁺ were prepared and characterized by elemental analyses, magnetic moments and spectral studies. SCA acts as a uninegatively charged bidentate ligand and reacts with the metal ion via the oxygen atom of the secondary unacetylated hydroxyl group in the glucose subunit of the polymer, plus the oxygen atom of the vicinal ester group, to form a five-membered chelate ring.