exhibits extensive first pass metabolism with poor oral bioavailability (27%–50%) limiting its therapeutic efficiency. The present study involved an attempt to enhance its aqueous solubility by formulating as solid dispersions (SDs) using sodium starch glycollate (SSG) as a carrier. The dispersions were formulated by dispersion method and evaluated by phase solubility, drug content, in vitro release and mathematical modelling. Solid state characterisation of samples was carried out by X-ray diffraction (XRD), differential scanning calorimetric (DSC), Fourier transform infrared spectrophotometry (FTIR), near infrared (NIR), Raman analysis and wettability studies. The phase solubility and thermodynamic parameters indicated the spontaneity and solubilisation effect of carrier. The release rate from the dispersions was higher than pure drug and found to increase with an increase in carrier content. The optimised dispersions were selected based on release studies, profiles and dissolution parameters. XRD, DSC, FTIR, NIR and Raman analysis proved the crystallinity reduction, changes in crystal quality and compatibility between drug and carriers. Wettability studies proved the increased wettability in selected dispersions. Based on the findings, possible mechanisms that would have contributed to dissolution enhancement of CLZ were suggested. Such findings could be extrapolated to enhance the aqueous solubility of other poorly water-soluble drugs.
Many attempts have been focused in the past on preparing of synthetic E-tricalcium (E-TCP), which being employed as bone substitute due to its biocompatibility and resorbability. Low temperature synthesize such as sol-gel method become popular due to the high product purity and homogenous composition. Sol-gel method is less economical towards commercialization because the cost of raw materials and the yield of the product that can be achieved. This paper describes the synthesis of ETCP via mixing of CaCO3 and H3PO4 followed by calcinations process at 750qC – 1050qC. X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimeter (DSC), fourier transformation infra-red (FTIR) were used for characterization and evaluation of the phase composition, morphology, particle size and thermal behavior of the product. E-TCP phase start to occur after calcinations at 750qC.
Differential scanning calorimetry (DSC) is developed and used for detection of butter adulteration with lard. Butter has the similar characteristics to lard makes lard a desirable adulterant in butter. DSC provides unique thermal profiling for lard and butter. In the heating thermogram of the mixture, there was one major endothermic peak (peak A) with a smaller shoulder peak embedded in the major peak that gradually smoothed out to the major peak as the lard percent increased. In the cooling thermogram, there were one minor peak (peak B) and two major exothermic peaks, peak C which increased as lard percent increased and peak D which decreased in size as the lard percent increased. From Stepwise Multiple Linear Regression (SMLR) analysis, two independent variables were found to be able to predict lard percent adulteration in butter with R2 (adjusted) of 95.82. The SMLR equation of lard percent adulteration in butter is 293.1 - 11.36 (Te A) - 2.17 (Tr D); where Te A is the endset of peak A and Tr D is the range of thermal transition for peak D. These parameters can serve as a good measurement parameter in detecting lard adulteration in butter. DSC is a very useful means for halal screening technique to enhance the authenticity of Halal process.
A study was carried out to compare the composition and thermal profiles of the fat component of six brands of commercial biscuits (BA, BB, BC, BD, BE & BF) with those of lard and palm oil. Extraction of fat from biscuit samples was done using petroleum ether according to the soxhlet extraction procedure. The isolated fat samples along with lard and palm oil were analyzed using gas liquid chromatography (GLC), reversed-phase high performance liquid chromatography (RP-HPLC), and differential scanning calorimetry (DSC). According to GLC analysis, palm oil, lard and all six biscuit brands had either palmitic or oleic acid as major fatty acids. Sn-2 positional analysis of fatty acids showed that oleic (> 60%) as the most dominant fatty acid of palm oil and biscuit brands BA, BB, BC, and BD while palmitic (> 60%) as the most dominant fatty acid of lard and biscuit brands BE and BF. RP-HPLC analysis showed that the triacylglycerol (TAG) profiles of lard and biscuit brands BE and BF were closely similar while those of brands BA, BB, BC, and BD and palm oil were similar. DSC analysis showed that the cooling and heating profiles of lard and brands BE and BF were similar, while those of palm oil and brands BA, BB, BC, and BD were similar. Hence, this study concluded that biscuit brands BE and BF are not suitable for consumers whose religious restriction prohibit the use of lard as food ingredient.
Crystallinity plays a vital role in the pharmaceutical industry. It affects drug manufacturing, development processes, and the stability of pharmaceutical dosage forms. An objective of this study was to measure and analyze the carbamazepine (CBZ) crystallinity before and after formulation. Moreover, it intended to determine the extent to which the crystallinity of CBZ would affect the drug loading, the particle size, and the release of CBZ from the microparticles. The CBZ microparticles were prepared by encapsulating CBZ in ethyl cellulose (EC) polymer using a solvent evaporation method. EC was used here as a release modifier polymer and polyvinyl alcohol (PVA) as an aqueous phase stabilizer. Factorial design was used to prepare the CBZ microparticle formulations, including polymer concentration, solvent (dichloromethane, ethyl acetate), PVA concentrations factor, the homogenization time, and homogenization speed. The crystallinity of CBZ was calculated utilizing differential scanning calorimetry (DSC) thermal analysis. The crystallinity was calculated from the enthalpy of CBZ. Enthalpy was analyzed from the area under the curve peak of CBZ standard and CBZ-loaded microparticles. DSC and ATR-FTIR assessed the possible interaction between CBZ and excipients in the microparticle. The prepared CBZ microparticles showed various changes in the crystallinity rate of CBZ. The changes in the rate of CBZ crystallinity had different effects on the particle size, the drug loading, and the release of CBZ from the polymer. Statistically, all studied factors significantly affected the crystallinity of CBZ after formulation to microparticles.
In this study, we fabricated a modified biomaterial based on chitosan and gelatin, which is an intrinsic hydrophilic membrane for oil-water separation to clean water contamination by oil. Modification of the membrane with a non-toxic natural crosslinker, genipin, significantly enhanced the stability of the biopolymer membrane in a water-based medium towards an eco-friendly environment. The effects of various compositions of genipin-crosslinked chitosan-gelatin membrane on the rheological properties, thermal stability, and morphological structure of the membrane were investigated using a dynamic rotational rheometer, thermogravimetry analysis, and chemical composition by attenuated total reflectance spectroscopy (ATR). Modified chitosan-gelatin membrane showed completely miscible blends, as determined by field-emission scanning electron microscopy, differential scanning calorimetry, and ATR. Morphological results showed membrane with establish microstructure to further experiment as filtration product. The membranes were successfully tested for their oil-water separation efficiencies. The membrane proved to be selective and effective in separating water from an oil-water mixture. The optimum results achieved a stable microporous structure of the membrane (microfiltration) and a separation efficiency of above 98%. The membrane showed a high permeation flux, generated as high as 698 and 420 L m-2 h-1 for cooking and crude oils, respectively. Owing to its outstanding recyclability and anti-fouling performance, the membrane can be washed away easily, ensuring the reusability of the prepared membrane.
Star-shaped polymers have vast potential in bioapplication due to their architecture. In this study, the suitability of ring opening polymerization (ROP) technique to synthesis star-shaped poly(caprolactone) and the thermal properties of the synthesized star-shaped polymers were demonstrated. The 4 -arm star- shaped of poly(caprolactone) (4s PCL) with -OH terminal and average molecular weight (Mn) of 5000, 10000, and 15000 g/mol were synthesized via ROP of ԑ-caprolactone (ԑ-CL) using a symmetric pentaerythritol (PET) as the core. Different molecular weights were obtained by using different ratios of ԑ-CL and PET in the presence of catalyst, stannous octoate (Sn(Oct)2). The FTIR spectra showed the presence of bands of methylene group of polymer repeating chain which confirm ROP of the ԑ- caprolactone. The average molecular weight (Mn) determined from proton nuclear magnetic resonance (1H NMR) analysis showed that all 4s PCL have approximately the same molecular weight as the theoretical values. All polymers obtained had high yield with >85%. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis showed that there were no significance different in the thermal properties of the synthesized polymers. A single step degradation for all 4s PCL was observed and the crystallization melting point of the polymers was within the range of melting point of PCL.
This study was to characterize the seed fat from Madhuca longifolia known as Mee fat and its solid and liquid fractions with the objective of distinguishing them. A sample of Mee fat was partitioned into solid and liquid fractions using acetone as the solvent medium. The isolated fractions were compared to the native Mee fat sample with respect to various physico-chemical parameters using standard chemical methods as well as instrumental techniques such as, gas liquid chromatography (GLC), reversed-phase high performance liquid chromatography (RP-HPLC), and differential scanning calorimetry (DSC). Basic analyses indicated that there were wide variations between the native sample and its fractions with respect to iodine value (IV), and slip melting point (SMP). The cloud point (CP) of the liquid fraction was found to be 10.5 degrees C. Fatty acid compositional analyses showed that the proportion of saturated fatty acids (SFA) such as palmitic and stearic went up in the high-melting fraction (HMF) while in low-melting fraction (LMF) the proportion of unsaturated fatty acid (USFA) such as oleic and lenoleic increased. According to the HPLC analyses, Mee fat had a tiacyl glycerol (TAG) sequence similar to that of palm oil. After fractionation, the solid and liquid fractions obtained were found to have TAG profiles very much different from the native sample. Thermal analyses by DSC showed that Mee fat had two-widely separated high and low melting thermal transitions, a feature which was beneficial for the effective separation of solid and liquid fractions. The thermal profiles displayed by the fractions were clearly distinguishable from that of the native sample.
This study adopts Differential Scanning Calorimetry (DSC) to analyze the thermal properties of samples (2.5-4.0 mg) from the tip, middle, and base sections of individual paracetamol suppositories, which were sampled carefully using a stainless steel scalpel. The contents of paracetamol present in the samples obtained from these sections were determined from the enthalpies of fusion of paracetamol and expressed as % w/w paracetamol to allow comparison of the amount of paracetamol found in each section. The tip, middle, and base sections contained 10.1+/-0.2%, 10.1+/-0.2%, and 10.3+/-0.2% w/w paracetamol, and are statistically similar (One-way anova; p>0.05). This indicates that the preparation technique adopted produces high quality suppositories in terms of content uniformity. The contents of paracetamol in the 120-mg paracetamol suppositories determined by DSC and UV spectrophotometry were statistically equivalent (Students's t-test; p>0.05), 120.8+/-2.6 mg and 120.8+/-1.5 mg, respectively, making DSC a clear alternative method for the measurement of content of drug in suppositories. The main advantages of the method are that samples of only 2.5-4.0 mg are required and the procedure does not require an extraction process, which allows for the analysis to be completed rapidly. In addition, it is highly sensitive and reproducible, with the lower detection limit at 4.0% w/w paracetamol, which is about 2.5 times lower than the content of paracetamol (10% w/w) present in our 120-mg paracetamol suppositories and commercial paracetamol suppositories, which contained about 125 mg paracetamol. Therefore, this method is particularly suited for determination of content uniformity in individual suppositories in quality control (QC) and in process quality control (PQC).
The aim of this study was to evaluate the effect of powder-to-liquid ratio on the glass transition temperature (Tg) and the tensile properties of denture base material prepared from poly (methyl methacrylate) (PMMA) and hydroxyapatite (HA) previously treated with 3-trimethoxysilylpropyl methacrylate (gamma-MPS). Specimens for mechanical testing were prepared by adding composites powder (PMMA, BPO and HA) to the monomer (MMA and EGDMA) followed by hand mixing as in dental laboratory description usage. The glass transition temperature was studied by using differential scanning calorimetry (DSC). It was observed that the tensile properties and the Tg were affected by the powder-to-liquid ratio. The mechanical characterization of the materials were performed by using single edge notch-tension (SEN-T) specimens; the fracture toughness was slightly higher in formulation which contained HA filler compared to commercial denture base material.
A series of new mesogenic azomethine diols were successfully synthesized by condensation reactions between various chloroalkanols and N,N'-bis(4-hydroxy)-benzylidene-o-toluidine (1). The structures of these compounds were confirmed by CHN, FT-IR, (1)H-NMR, and (13)C-NMR spectrophotometer. Their thermotropic liquid crystalline behavior was studied using differential scanning calorimetry (DSC) and polarizing optical microscope (POM). 4,4'-di(4-Hydroxybutoxy)-N-benzylidine-o-tolidine (2a) does not exhibit liquid crystalline properties. A nematic texture was observed for mesogenic diols 2b, and 2d, whereas the diol 2c exhibits a smectic mesophase. The increase of terminal alkyl chain in these mesogenic diols leads to a decrease in the transition temperature.
Plasticized poly(lactic acid) PLA with epoxidized vegetable oils (EVO) were prepared using a melt blending method to improve the ductility of PLA. The plasticization of the PLA with EVO lowers the Tg as well as cold-crystallization temperature. The tensile properties demonstrated that the addition of EVO to PLA led to an increase of elongation at break, but a decrease of tensile modulus. Plasticized PLA showed improvement in the elongation at break by 2058% and 4060% with the addition of 5 wt % epoxidized palm oil (EPO) and mixture of epoxidized palm oil and soybean oil (EPSO), respectively. An increase in the tensile strength was also observed in the plasticized PLA with 1 wt % EPO and EPSO. The use of EVO increases the mobility of the polymeric chains, thereby improving the flexibility and plastic deformation of PLA. The SEM micrograph of the plasticized PLA showed good compatible morphologies without voids resulting from good interfacial adhesion between PLA and EVO. Based on the results of this study, EVO may be used as an environmentally friendly plasticizer that can improve the overall properties of PLA.
The D-optimal mixture experimental design was employed to optimize the melting point of natural lipstick based on pitaya (Hylocereus polyrhizus) seed oil. The influence of the main lipstick components-pitaya seed oil (10%-25% w/w), virgin coconut oil (25%-45% w/w), beeswax (5%-25% w/w), candelilla wax (1%-5% w/w) and carnauba wax (1%-5% w/w)-were investigated with respect to the melting point properties of the lipstick formulation. The D-optimal mixture experimental design was applied to optimize the properties of lipstick by focusing on the melting point with respect to the above influencing components. The D-optimal mixture design analysis showed that the variation in the response (melting point) could be depicted as a quadratic function of the main components of the lipstick. The best combination of each significant factor determined by the D-optimal mixture design was established to be pitaya seed oil (25% w/w), virgin coconut oil (37% w/w), beeswax (17% w/w), candelilla wax (2% w/w) and carnauba wax (2% w/w). With respect to these factors, the 46.0 °C melting point property was observed experimentally, similar to the theoretical prediction of 46.5 °C. Carnauba wax is the most influential factor on this response (melting point) with its function being with respect to heat endurance. The quadratic polynomial model sufficiently fit the experimental data.
Physicochemical properties of threadfin bream surimi with different levels of polydextrose (3%, 6%, 9% and 12%), raw surimi, raw surimi with addition sodium tripolyphosphate and commercial surimi (sucrose) during 6 months of frozen storage were investigated. The analyses included the measurement of Ca(2+)-ATPase, sulfhydryl contents, protein solubility, sodium dodecyl sulfate polyacrylamide gel electrophoresis, differential scanning calorimetry and scanning electron microscopy. The Ca(2+)-ATPase, sulfhydryl content and protein solubility levels added with 3%, 6%, 9% and 12% polydextrose can be maintained until the 6 months of storage by 47.33%, 41.60% and 51.41%, respectively. Differential scanning calorimetry showed decreases in thermal stabilization of myosin with regard to transition termperature. Analysis by scanning electron microscopy demonstrated that the number of pores formed was increased after storage. This study suggested that surimi stored with the polydextrose as a cryoprotectant was able to maintain physicochemical of surimi better compared to raw surimi with no additives or raw surimi with sodium tripolyphosphate.
The aim of this study was to enhance the dissolution rate of efavirenz using solid dispersion systems (binary and ternary). A comparison between solvent and fusion method was also investigated. Solid dispersions of efavirenz were prepared using polyethylene glycol 8000, polyvinylpyrrolidone K30 alone and combination of both. Tween 80 was incorporated to obtain a ternary solid dispersion system. Dissolution tests were conducted and evaluated on the basis of cumulative percentage drug release and dissolution efficiency. Physicochemical characterizations of the solid dispersions were carried out using differential scanning calorimetric, powder X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. Dissolution was remarkably improved in both systems compared to pure efavirenz (P<0.05). An optimum ratio was identified at a drug:polymer of 1:10. Incorporation of Tween 80 to 1:10 formulations formed using solvent method showed further improvement in the dissolution rate. Physicochemical characterization results suggested that efavirenz existed in the amorphous form in all the solid dispersion systems providing evidence of improvement in dissolution. No statistically significant difference (P>0.05) in dissolution was observed between the two methods. Binary and ternary solid dispersion systems both have showed a significant improvement in the dissolution rate of efavirenz. Formulations with only polyvinylpyrrolidone K30 showed best dissolution profile and 1:10 was identified as an optimum drug-polymer weight ratio.
Triethoxyphenylsilane (TEPS)-functionalized magnetic palm-based powdered activated carbon (MPPAC-TEPS) was prepared and characterized using various spectroscopic methods, and then tested for the removal of bisphenol A, carbamazepine, ibuprofen and clofibric acid. Magnetite film on MPPAC-TEPS was homogeneously coated on the outer surface of palm-based powdered activated carbon (PPAC) through a hydrothermal co-precipitation technique. Followed by silanization of phenyl-functionalized organosilane on MPPAC's magnetic film. As results, micro/mesopore surface area and volume increased without significant pore clogging and iron (Fe) dissolution under the acidic conditions was greatly decreased. The unique structural and chemical features of MPPAC-TEPS were found to be the main reasons for the enhanced adsorption rates and removal capacities of POPs. The presence of electrolytes and different pH values greatly affected the sorption efficiencies. The dominant sorption mechanism of POPs by MPPAC-TEPS was determined to be π-π interaction (physisorption), based on thermodynamic (ΔG°) and differential scanning calorimetry (DSC). Thermal regeneration at a low temperature (350 °C) was an effective method to desorb the retained POPs and enabled to reactivate MPPAC-TEPS with sustained sorption rates and capacities, whereas PPAC was largely exhausted. As a new type of sorbent for POPs, MPPAC-TEPS has operational advantages, such as magnetic separation and stable regeneration.
Gel polymer electrolytes using imidazolium based ionic liquids have attracted much attention in dye-sensitized solar cell applications. Hydroxypropyl cellulose (HPC), sodium iodide (NaI), 1-methyl-3-propylimidazolium iodide (MPII) as ionic liquid (IL), ethylene carbonate (EC) and propylene carbonate (PC) are used for preparation of non-volatile gel polymer electrolyte (GPE) system (HPC:EC:PC:NaI:MPII) for dye-sensitized solar cell (DSSC) applications. The highest ionic conductivity of 7.37 × 10(-3) S cm(-1) is achieved after introducing 100% of MPII with respect to the weight of HPC. Temperature-dependent ionic conductivity of gel polymer electrolytes is studied in this work. XRD patterns of gel polymer electrolytes are studied to confirm complexation between HPC polymer, NaI and MPII. Thermal behavior of the GPEs is studied using simultaneous thermal analyzer (STA) and differential scanning calorimetry (DSC). DSSCs are fabricated using gel polymer electrolytes and J-V centeracteristics of fabricated dye sensitized solar cells were analyzed. The gel polymer electrolyte with 100 wt.% of MPII ionic liquid shows the best performance and energy conversion efficiency of 5.79%, with short-circuit current density, open-circuit voltage and fill factor of 13.73 mA cm(-2), 610 mV and 69.1%, respectively.
Poor solubility and bioavailability of drugs are often affected by its microscopic structural properties. Nitrofurantoin (NF), a Biopharmaceutics Classification System class II item, has a low water solubility with low plasma concentrations. To improve its therapeutic efficacy, formulation strategy of solid dispersion (SD) and co-crystallization are compared herein. The co-crystal is prepared with citric acid in 1:1 stoichiometric ratio while SD consists of 30% w/w nitrofurantoin and 70% w/w hydroxypropyl methylcellulose (HPMC) as the carrier system. As a control, the physical mixture of NF and HPMC was prepared. All the preparations were characterized with differential scanning calorimetry (DSC), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), microscopy analysis, solubility, and dissolution studies. The formation of co-crystal, solvent evaporated, and spray-dried SD are confirmed by the ATR-FTIR where peaks shifting of several functional groups indicate the formation of the hydrogen bond. Dissolution studies showed a greater initial dissolution rate in co-crystal than SD despite the possible presence of amorphous content in the SD system. Overall, co-crystal is concluded to be a better approach than SD for an effective dissolution.
Polymer electrolyte membranes based on the natural polymer κ-carrageenan were modified and characterized for application in electrochemical devices. In general, pure κ-carrageenan membranes show a low ionic conductivity. New membranes were developed by chemically modifying κ-carrageenan via phosphorylation to produce O-methylene phosphonic κ-carrageenan (OMPC), which showed enhanced membrane conductivity. The membranes were prepared by a solution casting method. The chemical structure of OMPC samples were characterized using Fourier transform infrared spectroscopy (FTIR), 1H nuclear magnetic resonance (1H NMR) spectroscopy and 31P nuclear magnetic resonance (31P NMR) spectroscopy. The conductivity properties of the membranes were investigated by electrochemical impedance spectroscopy (EIS). The characterization demonstrated that the membranes had been successfully produced. The ionic conductivity of κ-carrageenan and OMPC were 2.79 × 10-6 S cm-1 and 1.54 × 10-5 S cm-1, respectively. The hydrated membranes showed a two orders of magnitude higher ionic conductivity than the dried membranes.
The demands for applicable tissue-engineered scaffolds that can be used to repair load-bearing segmental bone defects (SBDs) is vital and in increasing demand. In this study, seven different combinations of 3 dimensional (3D) novel nanocomposite porous structured scaffolds were fabricated to rebuild SBDs using an extraordinary blend of cockle shells (CaCo3) nanoparticles (CCN), gelatin, dextran and dextrin to structure an ideal bone scaffold with adequate degradation rate using the Freeze Drying Method (FDM) and labeled as 5211, 5400, 6211, 6300, 7101, 7200 and 8100. The micron sized cockle shells powder obtained (75 µm) was made into nanoparticles using mechano-chemical, top-down method of nanoparticles synthesis with the presence of the surfactant BS-12 (dodecyl dimethyl bataine). The phase purity and crystallographic structures, the chemical functionality and the thermal characterization of the scaffolds' powder were recognized using X-Ray Diffractometer (XRD), Fourier transform infrared (FTIR) spectrophotometer and Differential Scanning Calorimetry (DSC) respectively. Characterizations of the scaffolds were assessed by Scanning Electron Microscopy (SEM), Degradation Manner, Water Absorption Test, Swelling Test, Mechanical Test and Porosity Test. Top-down method produced cockle shell nanoparticles having averagely range 37.8±3-55.2±9 nm in size, which were determined using Transmission Electron Microscope (TEM). A mainly aragonite form of calcium carbonate was identified in both XRD and FTIR for all scaffolds, while the melting (Tm) and transition (Tg) temperatures were identified using DSC with the range of Tm 62.4-75.5 °C and of Tg 230.6-232.5 °C. The newly prepared scaffolds were with the following characteristics: (i) good biocompatibility and biodegradability, (ii) appropriate surface chemistry and (iii) highly porous, with interconnected pore network. Engineering analyses showed that scaffold 5211 possessed 3D interconnected homogenous porous structure with a porosity of about 49%, pore sizes ranging from 8.97 to 337 µm, mechanical strength 20.3 MPa, Young's Modulus 271±63 MPa and enzymatic degradation rate 22.7 within 14 days.