Abstract: Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.
Abstract: A precise, sensitive, rapid and selective method for the solvent extraction, spectrophotometric determination of palladium(II) using para-methylphenyl thiourea (PMPT) as an extractant is developed. Palladium(II) forms yellow colored complex with PMPT which shows an absorption maximum at 300 nm. The colored complex obeys Beer’s law up to 7.0 µg ml-1 of palladium. The molar absorptivity and Sandell’s sensitivity were found to be 8.486 x 103 l mol-1cm-1 and 0.0125 μg cm-2 respectively. The optimum conditions for the extraction and determination of palladium have been established by monitoring the various experimental parameters. The precision of the method has been evaluated and the relative standard deviation has been found to be less than 0.53%. The proposed method is free from interference from large number of foreign ions. The method has been successfully applied for the determination of palladium from alloy, synthetic mixtures corresponding to alloy samples.
Abstract: Environmental and sustainability concerns push the industries to manufacture alternative materials having less environmental impact. The Wood Plastic Composites (WPCs) produced by blending the biopolymers and natural fillers permit not only to tailor the desired properties of materials but also are the solution to meet the environmental and sustainability requirements. This work presents the elaboration and characterization of the fully green WPCs prepared by blending a biopolymer, BIOPLAST® GS 2189 and spruce sawdust used as filler with different amounts. Since both components are bio-based, the resulting material is entirely environmentally friendly. The mechanical, thermal, structural properties of these WPCs were characterized by different analytical methods like tensile, flexural and impact tests, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and X-ray Diffraction (XRD). Their water absorption properties and resistance to the termite and fungal attacks were determined in relation with different wood filler content. The tensile and flexural moduli of WPCs increased with increasing amount of wood fillers into the biopolymer, but WPCs became more brittle compared to the neat polymer. Incorporation of spruce sawdust modified the thermal properties of polymer: The degradation, cold crystallization, and melting temperatures shifted to higher temperatures when spruce sawdust was added into polymer. The termite, fungal and water absorption resistance of WPCs decreased with increasing wood amount in WPCs, but remained in durability class 1 (durable) concerning fungal resistance and quoted 1 (attempted attack) in visual rating regarding to the termites resistance except that the WPC with the highest wood content (30 wt%) rated 2 (slight attack) indicating a long term durability. All the results showed the possibility to elaborate the easy injectable composite materials with adjustable properties by incorporation of BIOPLAST® GS 2189 and spruce sawdust. Therefore, lightweight WPCs allow both to recycle wood industry byproducts and to produce a full ecologic material.
Abstract: Introduction: The application of fissure sealants is considered to be an important primary prevention method used in dental medicine. However, the formation of microleakage gaps between tooth enamel and the fissure sealant applied is one of the most common reasons of dental caries development in teeth with fissure sealants. The association between various dental biomaterials may limit the major disadvantages and limitations of biomaterials functioning in a complementary manner. The present study consists in the incorporation of a cariostatic agent – silver diamine fluoride (SDF) – in a resin-based fissure sealant followed by the study of release kinetics by spectrophotometry analysis of the association between both biomaterials and assessment of the inhibitory effect on the growth of the reference bacterial strain Streptococcus mutans (S. mutans) in an in vitro study. Materials and Methods: An experimental in vitro study was designed consisting in the entrapment of SDF (Cariestop® 12% and 30%) into a commercially available fissure sealant (Fissurit®), by photopolymerization and photocrosslinking. The same sealant, without SDF was used as a negative control. The effect of the sealants on the growth of S. mutans was determined by the presence of bacterial inhibitory halos in the cultures at the end of the incubation period. In order to confirm the absence of bacteria in the surface of the materials, Scanning Electron Microscopy (SEM) characterization was performed. Also, to analyze the release profile of SDF along time, spectrophotometry technique was applied. Results: The obtained results indicate that the association of SDF to a resin-based fissure sealant may be able to increase the inhibition of S. mutans growth. However, no SDF release was noticed during the in vitro release studies and no statistical significant difference was verified when comparing the inhibitory halo sizes obtained for test and control group. Conclusions: In this study, the entrapment of SDF in the resin-based fissure sealant did not potentiate the antibacterial effect of the fissure sealant or avoid the immediate development of dental caries. The development of more laboratorial research and, afterwards, long-term clinical data are necessary in order to verify if this association between these biomaterials is effective and can be considered for being used in oral health management. Also, other methodologies for associating cariostatic agents and sealant should be addressed.
Abstract: One of the most important factors for air pollution is that the concentrations of PM10 maintain a constant trend, with the exception of some places where that frequently surpasses the allowed ranges established by Colombian legislation. The community that surrounds the Universidad Libre Bogotá is inhabited by a considerable number of students and workers, all of whom are possibly being exposed to PM10 for long periods of time while on campus. Thus, the chemical characterization of PM10 found in the ambient air at the Universidad Libre Bogotá was identified as a problem. A Hi-Vol sampler and EPA Test Method 5 were used to determine if the quality of air is adequate for the human respiratory system. Additionally, quartz fiber filters were utilized during sampling. Samples were taken three days a week during a dry period throughout the months of November and December 2015. The gravimetric analysis method was used to determine PM10 concentrations. The chemical characterization includes non-conventional carcinogenic pollutants. Atomic absorption spectrophotometry (AAS) was used for the determination of metals and VOCs were analyzed using the FTIR (Fourier transform infrared spectroscopy) method. In this way, concentrations of PM10, ranging from values of 13 µg/m3 to 66 µg/m3, were obtained; these values were below standard conditions. This evidence concludes that the PM10 concentrations during an exposure period of 24 hours are lower than the values established by Colombian law, Resolution 610 of 2010; however, when comparing these with the limits set by the World Health Organization (WHO), these concentrations could possibly exceed permissible levels.
Abstract: Three polyvinyl chloride membrane sensors were developed for the electrochemical evaluation of ferrous, manganese and zinc ions. The sensors were used for assaying metal ions in cervical mucus (CM) of Egyptian river buffalo-cows (Bubalus bubalis) as their levels vary dependent on cyclical hormone variation during different phases of estrus cycle. The presented sensors are based on using ionophores, β-cyclodextrin (β-CD), hydroxypropyl β-cyclodextrin (HP-β-CD) and sulfocalix-4-arene (SCAL) for sensors 1, 2 and 3 for Fe2+, Mn2+ and Zn2+, respectively. Dioctyl phthalate (DOP) was used as the plasticizer in a polymeric matrix of polyvinylchloride (PVC). For increasing the selectivity and sensitivity of the sensors, each sensor was enriched with a suitable complexing agent, which enhanced the sensor’s response. For sensor 1, β-CD was mixed with bathophenanthroline; for sensor 2, porphyrin was incorporated with HP-β-CD; while for sensor 3, oxine was the used complexing agent with SCAL. Linear responses of 10-7-10-2 M with cationic slopes of 53.46, 45.01 and 50.96 over pH range 4-8 were obtained using coated graphite sensors for ferrous, manganese and zinc ionic solutions, respectively. The three sensors were validated, according to the IUPAC guidelines. The obtained results by the presented potentiometric procedures were statistically analyzed and compared with those obtained by atomic absorption spectrophotometric method (AAS). No significant differences for either accuracy or precision were observed between the two techniques. Successful application for the determination of the three studied cations in CM, for the purpose to determine the proper time for artificial insemination (AI) was achieved. The results were compared with those obtained upon analyzing the samples by AAS. Proper detection of estrus and correct time of AI was necessary to maximize the production of buffaloes. In this experiment, 30 multi-parous buffalo-cows were in second to third lactation and weighting 415-530 kg, and were synchronized with OVSynch protocol. Samples were taken in three times around ovulation, on day 8 of OVSynch protocol, on day 9 (20 h before AI) and on day 10 (1 h before AI). Beside analysis of trace elements (Fe2+, Mn2+ and Zn2+) in CM using the three sensors, the samples were analyzed for the three cations and also Cu2+ by AAS in the CM samples and blood samples. The results obtained were correlated with hormonal analysis of serum samples and ultrasonography for the purpose of determining of the optimum time of AI. The results showed significant differences and powerful correlation with Zn2+ composition of CM during heat phase and the ovulation time, indicating that the parameter could be used as a tool to decide optimal time of AI in buffalo-cows.
Abstract: A simple, accurate and precise direct spectrophotometric method has been developed for the determination of cefixime in tablets and capsules. The method is based on the reaction of cefixime with a mixture of potassium iodide and potassium iodate to form yellow coloured product in ethanol-distilled water medium at room temperature which absorbed maximally at 352 nm. The factors affecting the reaction product were carefully studied and optimized. The validation parameters based on International Conference on Harmonisation (ICH, USA) guidelines were followed. The effect of common excipients used as additives has been tested and the tolerance limit was calculated for the determination of cefixime. Beer’s law is obeyed in the concentration range of 4 – 24 ug mL-1 with apparent molar absorptivity of 1.52 × 104 L mol-1cm-1 and Sandell’s sensitivity of 0.033 ug/cm2/ 0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.32 and 1.06 ug mL-1, respectively. The proposed method has been successfully applied for the determination of cefixime in pharmaceutical formulations. The results obtained by the proposed method were statistically compared with the reference method using t- and F- values and found no significant difference between the two methods. The proposed method can be used as an alternate method for routine quality control analysis of cefixime in pharmaceutical formulations.
Abstract: Natural dye extracted from Caesalpinia sappan Linn. was applied to a cotton fabric and silk yarn by dyeing process. The dyestuff component of Caesalpinia sappan Linn. was extracted using water and ethanol. Analytical studies such as UV–VIS spectrophotometry and gravimetric analysis were performed on the extracts. Brazilein, the major dyestuff component of Caesalpinia sappan Linn. was confirmed in both aqueous and ethanolic extracts by UV–VIS spectrum. The color of each dyed material was investigated in terms of the CIELAB (L*, a* and b*) and K/S values. Cotton fabric dyed without mordant had a shade of reddish-brown, while those post-mordanted with aluminum potassium sulfate, ferrous sulfate and copper sulfate produced a variety of wine red to dark purple color shades. Cotton fabric and silk yarn dyeing was studied using aluminum potassium sulfate as a mordant. The observed color strength was enhanced with increase in mordant concentration.
Abstract: The study realized on alive lambs in two different areas mountain and plain in Batna region, aims to demonstrate the possible effect of field type on cupric status of lambs, through evaluation of copper contents in the chain: soil – plant – animal by atomic absorption spectrophotometry. This comparative study also allowed the investigation of the influence of the age and the season. The results obtained show that contents of copper in the soil, forage in the same way as in the plasma of lambs are higher in the plain than in the mountainous area; however, the difference is significant only between the values of feed.
Abstract: Since nickel is a known toxic and carcinogenic metal, the present study was designed to evaluate the level of nickel released into the saliva of orthodontic patients. Non-stimulated saliva was collected from 18 patients attending The Orthodontic Clinic of Dental Faculty of Benghazi University. Patients were divided into two groups and level of nickel was determined by atomic absorption spectrophotometry. Nickel concentration value (mg/L) in first group prior to starting treatment was 0.097± 0.071. An increase in level of nickel was followed by decrease 4 and 8 weeks after applying the arch wire (0.208± 0.112) and (0.077±0.056 mg/L) respectively. Nickel levels in saliva of the second group were showed minimal variation and ranged from 0.061± 0.044mg/L to 0.083±0.054 throughout period of study. It may be concluded that there could be a release of nickel from the appliances used in first group but it doesn't reach toxic level in saliva.
Abstract: A spectrophotometric method was developed for simultaneous quantification of pseudoephedrine hydrochloride (PSE) triprolidine hydrochloride (TRI) using second derivative method (zero-crossing technique). The second derivative amplitudes of PSE and TRI were measured at 271 and 321 nm, respectively. The calibration curves were linear in the range of 200 to 1,000 g/ml for PSE and 10 to 50 g/ml for TRI. The method was validated for specificity, accuracy, precision, limit of detection and limit of quantitation. The proposed method was applied to the assaying and dissolution of PSE and TRI in commercial tablets without any chemical separation. The results were compared with those obtained by the official USP31 method and statistical tests showed that there is no significant between the methods at 95% confidence level. The proposed method is simple, rapid and suitable for the routine quality control application. KeywordsTriprolidine, Pseudoephedrine, Derivative spectrophotometry, Dissolution testing.
Abstract: Lutein is a dietary oxycarotenoid which is found
to reduce the risks of Age-related Macular Degeneration
(AMD). Supercritical fluid extraction of lutein esters from
marigold petals was carried out and was found to be much
effective than conventional solvent extraction. The
saponification of pre-concentrated lutein esters to produce free
lutein was studied which showed a composition of about 88%
total carotenoids (UV-VIS spectrophotometry) and 90.7%
lutein (HPLC). The lipase catalyzed hydrolysis of lutein esters
in conventional medium was investigated. The optimal
temperature, pH, enzyme concentration and water activity
were found to be 50°C, 7, 15% and 0.33 respectively and the
activity loss of lipase was about 25% after 8 times re-use in at
50°C for 12 days. However, the lipase catalyzed hydrolysis of
lutein esters in conventional media resulted in poor
conversions (16.4%).
Abstract: To unveil the mechanism of fast autooxidation of fish
myoglobins, the effect of temperature on the structural change of tuna
myoglobin was investigated. Purified myoglobin was subjected to
preincubation at 5, 20, 50 and 40oC. Overall helical structural decay
through thermal treatment up to 95oC was monitored by circular
dichroism spectrometry, while the structural changes around the heme
pocket was measured by ultraviolet/visible absorption spectrophotometry.
As a result, no essential structural change of myoglobin
was observed under 30oC, roughly equivalent to their body
temperature, but the structure was clearly damaged at 40oC. The Soret
band absorption hardly differed irrespective of preincubation
temperature, suggesting that the structure around the heme pocket was
not perturbed even after thermal treatment.
Abstract: The presence of heavy metals in the environment
could constitute a hazard to food security and public health. These
can be accumulated in aquatic animals such as fish. Samples of four
popular brands of canned fish in the Iranian market (yellowfin tuna,
common Kilka, Kawakawa and longtail tuna) were analyzed for level
of Cr after wet digestion with acids using graphite furnace atomic
absorption spectrophotometry. The mean concentrations for Cr in the
different brands were: 2.57, 3.24, 3.16 and 1.65 μg/g for brands A, B,
C and D respectively. Significant differences were observed in the Cr
levels between all of the different brands of canned fish evaluated in
this study. The Cr concentrations for the varieties of canned fishes
were generally within the FAO/WHO, U.S. FDA and U.S. EPA
recommended limits for fish.
Abstract: This paper presents a simple and sensitive kinetic
spectrophotometric method for the determination of ramipril in
commercial dosage forms. The method is based on the reaction of the
drug with 1-chloro-2,4-dinitrobenzene (CDNB) in dimethylsulfoxide
(DMSO) at 100 ± 1ºC. The reaction is followed
spectrophotometrically by measuring the rate of change of the
absorbance at 420 nm. Fixed-time (ΔA) and equilibrium methods are
adopted for constructing the calibration curves. Both the calibration
curves were found to be linear over the concentration ranges 20 - 220
μg/ml. The regression analysis of calibration data yielded the linear
equations: Δ A = 6.30 × 10-4 + 1.54 × 10-3 C and A = 3.62 × 10-4 +
6.35 × 10-3 C for fixed time (Δ A) and equilibrium methods,
respectively. The limits of detection (LOD) for fixed time and
equilibrium methods are 1.47 and 1.05 μg/ml, respectively. The
method has been successfully applied to the determination of ramipril
in commercial dosage forms. Statistical comparison of the results
shows that there is no significant difference between the proposed
methods and Abdellatef-s spectrophotometric method.