The effects of scanning rates (1, 5, 10 and 20 degrees C/min) on the DSC cooling profiles of 11 vegetable oils have been determined in order to monitor peak transition temperatures, onset temperatures and crystallisation enthalpies. Triacylglycerol (TAG) profiles and iodine value analyses were used to complement the DSC data. The melted samples exhibited complicated crystallising exotherms. As the cooling rate increased, the crystallisation temperature decreased and the breadth of the crystallisation exotherm on cooling from the melt increased. In addition, the intensity of the exothermic peak increased somewhat when the cooling rate was increased. At slow cooling rates, TAG had more time to interact. It is conceivable that, at a low cooling rate (1 degree C/min), a prominent exotherm would be observed on crystallisation of vegetable oils and fats. The occurrence of one exotherm upon cooling indicated the co-crystallisation of the TAG upon slow cooling. On the basis of the corollary results obtained, vegetable oils may be differentiated by their onset temperature (Ton) values in the DSC cooling curves. Generally, there was a shift of Ton toward lower values with increasing cooling rates.
The melting curves of 11 vegetable oils have been characterised. Vegetable oil samples that were cooled at a constant rate (5 degrees C/min) from the melt showed between one and seven melting endotherms upon heating at four different heating rates (1, 5, 10 and 20 degrees C/min) in a differential scanning calorimeter (DSC). Triacylglycerol (TAG) profiles and iodine value analyses were used to complement the DSC data. Generally, the melting transition temperature shifted to higher values with increased rates of heating. The breadth of the melting endotherm and the area under the melting peak also increased with increasing heating rate. Although the number of endothermic peaks was dependent on heating rate, the melting curves of the oil samples were not straightforward in that there was no correlation between the number of endothermic peaks and heating rates. Multiple melting behaviour in DSC experiments with different heating rates could be explained by: (1) the melting of TAG populations with different melting points; and (2) TAG crystal reorganisation effects. On the basis of the corollary results obtained, vegetable oils and fats may be distinguished from their offset-temperature (Toff) values in the DSC melting curves. The results showed that Toff values of all oil samples were significantly (p < 0.01) different in the melting curves scanned at four different scanning rates. These calorimetric results indicate that DSC is a valuable technique for studying vegetable oils.
The aim of this study was to evaluate the mechanical properties and glass transition temperature (Tg) of a denture base material prepared from high molecular weight poly methyl methacrylate (PMMA) and alumina (Al2O3). The glass transition temperature was studied by using differential scanning calorimetry (DSC). The effect of powder-to-liquid ratio was investigated. The result showed that the tensile properties and the Tg were slightly effected by the powder-to-liquid ratio. The ratio of 2.2:1 by weight of powder to liquid was found to be the best ratio for mixing the material to give the best result in this formulation.
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.
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).
Coating has been widely used in pharmaceutical manufacture either as non-functional or a functional entity. The objectives of the present study were to investigate the effect of plasticizers such as PEG400, PEG1000 and triacetin on mechanical properties, glass transition temperature and water vapor transmission of free films prepared from HPMC and/or HPMC:PVA blends, to develop suitable coating system for tablets, and to determine the release profiles of the coated tablets. The tensile strength of plasticized HPMC films was generally lower than that of control HPMC film and could be attributed to increased crystallinity and segmental chain mobility of HPMC. This effect increased as the concentration of plasticizer increased. Generally the addition of both grades of polyethylene glycol (PEG400 & PEG1000) increased the moisture permeability of HPMC films but the films containing triacetin provided a more rigid barrier to moisture compared to unplasticized HPMC films. The dissolution profiles of paracetamol tablets coated with 7% w/v HPMC coating-solutions containing PEG400, PEG1000 and triacetin, and those containing PEG400 & PVA together showed that HPMC had weak water resistance. The presence of PEG400 and 1000 in HPMC films further weakened its resistance to solubility while the presence of triacetin caused a little increase in HPMC water resistance. From the results it was concluded that HPMC at 7%w/w concentration was suitable for film-coating intended for non-functional coating. Presence of the PEG 400, PEG1000 and triacetin as well as the presence of PVA and PEG400 together improved the coating properties of HPMC films and made it more suitable as a non-functional coating material.
A polyglycolised glyceride carrier, Gelucire 50/13, was incorporated with paracetamol as a model drug, filled into hard gelatin capsules and stored at three different temperatures for various lengths of time. The resultant solidified matrix within the capsule was subjected to thermal analysis using differential scanning calorimetry (DSC) to ascertain its supramolecular structure. Polymorphic transformations towards more stable gelucire forms were observed upon aging the matrices, with samples stored at a temperature near the melting range of the lower temperature gelucire melting fraction showing the most profound changes. The increase in the rate of drug release from aged samples could be correlated to the alterations to the supramolecular structure of the gelucire. Accelerated drug release from aged samples could also be seen from in vivo studies using healthy human volunteers, although the extent of absorption was not affected. Therefore, even though the sustainability of release may be compromised by aging the gelucire matrices, the bioavailability of the incorporated drug is unlikely to be affected.
The applicability of microwave non-destructive testing (NDT) technique in characterization of matrix property of pharmaceutical films was investigated. Hydroxypropylmethylcellulose and loratadine were selected as model matrix polymer and drug, respectively. Both blank and drug loaded hydroxypropylmethylcellulose films were prepared using the solvent-evaporation method and were conditioned at the relative humidity of 25, 50 and 75% prior to physicochemical characterization using microwave NDT technique as well as ultraviolet spectrophotometry, differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR) techniques. The results indicated that blank hydroxypropylmethylcellulose film exhibited a greater propensity of polymer-polymer interaction at the O-H and C-H domains of the polymer chains upon conditioned at a lower level of relative humidity. In the case of loratadine loaded films, a greater propensity of polymer-polymer and/or drug-polymer interaction via the O-H moiety was mediated in samples conditioned at the lower level of relative humidity, and via the C-H moiety when 50% relative humidity was selected as the condition for sample storage. Apparently, the absorption and transmission characteristics of both blank and drug loaded films for microwave varied with the state of polymer-polymer and/or drug-polymer interaction involving the O-H and C-H moieties. The measurement of microwave NDT test at 8GHz was sensitive to the chemical environment involving O-H moiety while it was greatly governed by the C-H moiety in test conducted at a higher frequency band of microwave. Similar observation was obtained with respect to the profiles of microwave NDT measurements against the state of polymer-polymer and/or drug-polymer interaction of hydroxypropylmethylcellulose films containing chlorpheniramine maleate. The microwave NDT measurement is potentially suitable for use as an apparent indicator of the state of polymer-polymer and drug-polymer interaction of the matrix.
Effects of phosphorus content (510 to 987 ppm) on the gelatinization and retrogradation of 6 potato cultivars (Benimaru, Hokkaikogane, Irish Cobbler, Konafubuki, Sakurafubuki, and Touya) were studied. Pasting properties were analyzed by RVA, thermal properties by DSC, and mechanical properties of the starch gels by TA. Phosphorus was positively correlated with swelling power (r= 0.84) and negatively correlated with solubility (r= 0.83). Phosphorus content showed significant effect on certain pasting properties of potato starch such as peak viscosity, breakdown, and setback. Phosphorus content showed a significant positive correlation with peak viscosity (r= 0.95) and breakdown (r= 0.90). Increasing concentration of phosphorus tends to decrease the setback. Phosphorus content had no influence on thermal properties and mechanical properties of potato starch gel.
The drug release behavior of beads made of poly(methyl vinyl ether-co-maleic acid) was investigated with respect to the influence of microwave irradiation. The beads were prepared by an extrusion method with sodium diclofenac as a model water-soluble drug. The beads were subjected to microwave irradiation at 80 W for 5 and 20 min, and at 300 W for 1 min 20 s and 5 min 20 s. The profiles of drug dissolution, drug content, drug-polymer interaction, and polymer-polymer interaction were determined by using dissolution testing, drug content assay, differential scanning calorimetry, and Fourier transform infra-red spectroscopy. Keeping the level of supplied irradiation energy identical, treatment of beads by microwave at varying intensities of irradiation did not bring about similar drug release profiles. The extent and rate of drug released from beads were markedly enhanced through treating the samples by microwave at 80 W as a result of loss of polymer-polymer interaction via the (CH(2))(n) moiety, but decreased upon treating the beads by microwave at 300 W following polymer-polymer interaction via the O-H, COOH, and COO(-) moieties as well as drug-polymer interaction via the N-H, O-H, COO(-), and C-O moieties. The beads treated by microwave at 300 W exhibited a higher level of drug release retardation capacity than those that were treated by microwave at 80 W in spite of polymer-polymer interaction via the (CH(2))(n) moiety was similarly reduced in the matrix. The mechanism of drug release of both microwave-treated and untreated beads tended to follow zero order kinetics. The drug release was markedly governed by the state of polymer relaxation of the matrix and was in turn affected by the state of polymer-polymer and/or drug-polymer interaction in beads.
The capacity of microwave non-destructive testing (NDT) technique to characterize the matrix property of binary polymeric films for use as transdermal drug delivery system was investigated. Hydroxypropylmethylcellulose (HPMC) and polyethylene glycol (PEG) 3000 were the choice of polymeric matrix and plasticizer, respectively with loratadine as the model drug. Both blank and drug loaded HPMC-PEG 3000 films were prepared using the solvent-evaporation method. These films were conditioned at the relative humidity of 25, 50 and 75% prior to physicochemical characterization using the established methods of ultra-violet spectrophotometry, differential scanning calorimetry and Fourier transform infrared spectroscopy methods, as well as, novel microwave NDT technique. Blank films exhibited a greater propensity of polymer-polymer interaction at the O-H domain upon storage at a lower level of relative humidity, whereas drug loaded films exhibited a greater propensity of polymer-polymer, polymer-plasticizer and/or drug-polymer interaction via the O-H, C-H and/or aromatic C=C functional groups when they were stored at a lower or moderate level of relative humidity. The absorption and transmission characteristics of both blank and drug loaded films for microwave varied with the state of polymer-polymer, polymer-plasticizer, and/or drug-polymer interaction of the matrix. The measurements of microwave NDT test at 8 and 12 GHz were sensitive to the polar fraction of film involving functional group such as O-H moiety and the less polar environment of matrix consisting of functional groups such as C-H and aromatic C=C moieties. The state of interaction between polymer, plasticizer and/or drug of a binary polymeric film can be elucidated through its absorption and transmission profiles of microwave.
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.
The drug release characteristics of beads made of poly(methyl vinyl ether-co-maleic acid) using Zn2+ as the crosslinking agent were investigated with respect to the influence of microwave irradiation. The beads were prepared by an extrusion method with sodium diclofenac as a model water-soluble drug. They were subjected to microwave irradiation at 80W for 5 and 20 min, and at 300W for 1 min 20s and 5 min 20s. The profiles of drug dissolution, drug content, drug-polymer interaction and polymer-polymer interaction were determined by dissolution testing, drug content assay, differential scanning calorimetry and Fourier transform infrared spectroscopy. Treatment of beads by microwave at varying intensities of irradiation can aid to retard the drug release with a greater reduction extent through treating the beads for a longer duration of irradiation. The treatment of beads by microwave induced the formation of multiple polymeric domains of great strength and extent of polymer-polymer and drug-polymer interaction. The release of drug from beads was retarded via the interplay of O-H, N-H, C-H, (CH2)n and C-O functional groups of these domains, and was mainly governed by the state of polymer relaxation of the matrix unlike that of the untreated beads of which the release of drug was effected via drug diffusion and polymer relaxation. In comparison to Ca2+ crosslinked matrix which exhibited inconsistent drug release retardation behavior under the influence of microwave, the extent and rate of drug released from the Zn2+ crosslinked beads were greatly reduced by microwave and the release of drug from these beads was consistently retarded in response to both high and low intensity microwaves.
Synthetic polymers have attracted much attention in tissue engineering due to their ability to modulate biomechanical properties. This study investigated the feasibility of processing poly(epsilon-caprolactone) (PCL) homopolymer, PCL-poly(ethylene glycol) (PEG) diblock, and PCL-PEG-PCL triblock copolymers into three-dimensional porous scaffolds. Properties of the various polymers were investigated by dynamic thermal analysis. The scaffolds were manufactured using the desktop robot-based rapid prototyping technique. Gross morphology and internal three-dimensional structure of scaffolds were identified by scanning electron microscopy and micro-computed tomography, which showed excellent fusion at the filament junctions, high uniformity, and complete interconnectivity of pore networks. The influences of process parameters on scaffolds' morphological and mechanical characteristics were studied. Data confirmed that the process parameters directly influenced the pore size, porosity, and, consequently, the mechanical properties of the scaffolds. The in vitro cell culture study was performed to investigate the influence of polymer nature and scaffold architecture on the adhesion of the cells onto the scaffolds using rabbit smooth muscle cells. Light, scanning electron, and confocal laser microscopy showed cell adhesion, proliferation, and extracellular matrix formation on the surface as well as inside the structure of both scaffold groups. The completely interconnected and highly regular honeycomb-like pore morphology supported bridging of the pores via cell-to-cell contact as well as production of extracellular matrix at later time points. The results indicated that the incorporation of hydrophilic PEG into hydrophobic PCL enhanced the overall hydrophilicity and cell culture performance of PCL-PEG copolymer. However, the scaffold architecture did not significantly influence the cell culture performance in this study.
Gellan gum based floating beads containing clarithromycin (FBC) were prepared by iontotropic gelation method for stomach-specific drug delivery against Helicobacter pylori. The scanning electron microscope photograph indicated that prepared beads were spherical in shape with rough outer surface. Formulation variables such as concentrations of gellan, calcium carbonate and drug loading influenced the in vitro drug release characteristics of prepared beads. In vitro release rate of clarithromycin was corrected using first order degradation rate constant which is degraded significantly during the release study in simulated gastric fluid pH 2.0. Further, the absence of interactions between drug and polymer was confirmed by differential scanning calorimetry analysis. Kinetic treatment of the in vitro drug release data with different kinetic equations revealed matrix diffusion mechanism. Prepared beads showed good anti-microbial activity against isolated H. pylori strain. The prepared beads have shown good in vivo floating efficiency in rabbit stomach. The stability studies of beads did not show any significant changes after storage of beads at 40 degrees C/75% relative humidity for 6 months. The preliminary results from this study suggest that floating beads of gellan can be used to incorporate antibiotics like clarithromycin and may be effective when administered locally in the stomach against H. pylori.
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
Polyacrylamide (PAM), a commonly used organic synthetic flocculant, is known to have high reduction in turbidity treatment. However, PAM is not readily degradable. In this paper, pectin as a biopolymeric flocculant is used. The objectives are (i) to determine the characteristics of both flocculants (ii) to optimize the treatment processes of both flocculants in synthetic turbid waste water. The results obtained indicated that pectin has a lower average molecular weight at 1.63 x 10(5) and PAM at 6.00 x 10(7). However, the thermal degradation results showed that the onset temperature for pectin is at 165.58 degrees C, while the highest onset temperature obtained for PAM is at 235.39 degrees C. The optimum treatment conditions for the biopolymeric flocculant for flocculating activity was at pH 3, cation concentration at 0.55 mM, and pectin concentration at 3 mg/L. In contrast, PAM was at pH 4, cation concentration >0.05 mM and PAM concentration between 13 and 30 mg/L.
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.
Diacylglycerol (DAG), which has health-enhancing properties, is sometimes added to bakery shortening to produce baked products with enhanced physical functionality. Nevertheless, the quantity present is often too little to exert any positive healthful effects. This research aimed to produce bakery shortenings containing significant amounts of palm diacyglycerol (PDG). Physicochemical, textural and viscoelastic properties of the PDG bakery shortenings during 3 months storage were evaluated and compared with those of commercial bakery shortening (CS).
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.