Simple and sensitive spectrophotometric methods for the analysis of mesalamine in bulk and tablet dosage forms

Three simple, sensitive, economical and reproducible spectrophotometric methods (A, B and C) are described for determination of mesalamine in pure drug as well as in tablet dosage forms. Method A is based on the reduction of tungstate and/or molybdate in Folin Ciocalteu's reagent; method B describes the reaction between the diazotized drug and α-naphthol and method C is based on the reaction of the drug with vanillin, in acidic medium. Under optimum conditions, mesalamine could be quantified in the concentration ranges, 1-30, 1-15 and 2-30 µg mL-1 by method A, B and C, respectively. All the methods have been applied to the determination of mesalamine in tablet dosage forms. Results of analysis are validated statistically.

A validated HPLC analytical method for the analysis of solasonine and solamargine in in vitro skin penetration studies

To assess topical delivery studies of glycoalkaloids, an analytical method by HPLC-UV was developed and validated for the determination of solasonine (SN) and solamargine (SM) in different skin layers, as well as in a topical formulation. The method was linear within the ranges 0.86 to 990.00 µg/mL for SN and 1.74 to 1000.00 µg/mL for SM (r = 0.9996). Moreover, the recoveries for both glycoalkaloids were higher than 88.94 and 93.23% from skin samples and topical formulation, respectively. The method developed is reliable and suitable for topical delivery skin studies and for determining the content of SN and SM in topical formulations.

Development of a simple analytical method for determining trihalomethanes in beer using a headspace solid-phase microextraction technique

We developed a simple, rapid, and solventless method for analyzing trihalomethanes in beer samples using headspace solid-phase microextraction. The effects of varying experimental parameters, such as extraction temperature and time, addition of sodium chloride, and agitation speed, on extraction yield were studied using a univariate experimental design. Limits of detection between 0.22 and 0.46 µg L- 1 and wide linear ranges were achieved for trihalomethanes. We measured the trihalomethane recoveries and precision (as the standard deviation of repeat measurements) and demonstrated the applicability of the proposed method by analyzing 32 beer samples.

Análise de fármacos em águas por SPE-UPLC-ESI-MS/MS

A method was developed for the analysis of 31 pharmaceutical compounds in Lisbon's drinking water system, using solid-phase extraction (SPE) and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). The method was validated through estimation of the linearity range, method detection and quantification limits, matrix effects, precision and accuracy. The method detection and quantification limit ranges were 0.009-10 and 0.03-33 ng/L, respectively. Analytes were quantified in water samples collected from the EPAL (Empresa Portuguesa das Águas Livres S.A.) supply system. Carbamazepine, atenolol, sulfadiazine, sulfamethazine, sulfapyridine, sulfamethoxazole, acetaminophen, caffeine and erythromycin were quantified in the analysed samples.

Determinação simultânea de carbamazepina, fenitoína e fenobarbital em sangue seco em papel por cromatografia líquida de alta eficiência

Carbamazepine, phenobarbital and phenytoin were determined in dried blood spots (DBS) by high performance liquid chromatography, after extraction of 8 mm DBS using a mixture of acetonitrile and methanol. Analytes were separated by reversed-phase chromatography, with a run time of 17 minutes. Intra-assay and inter-assay precisions were in the 5.3 to 8.4% and 3.3 to 5.2% ranges, respectively. Accuracy was in the 98.8 to 104.3% range. The method had sensitivity to detect all analytes at levels below minimum therapeutic concentrations. The analytes were stable at 4 ºC and room temperature for up to 12 days and at 45 ºC for 9 days. The method was applied to 14 paired clinical samples of blood serum and DBS.

LC-MS/MS method applied to preclinical pharmacokinetic investigation of olanzapine-loaded lipid-core nanocapsules

In spite of different methods reported in the literature to determine olanzapine in biological fluids, all of them used high volumes of plasma. Therefore, the purpose of this paper was to develop an LC-MS/MS method using small plasma volume (0.1 mL) to apply in a preclinical pharmacokinetic investigation. The method was linear over the concentration ranges of 10 - 1000 ng mL-1. Extraction recoveries, stability, and validation parameters were evaluated. Results were within the acceptable limits of international guidelines. A significant decrease in clearance led to a significant 2.26-times increase in AUC0 - 6h of olanzapine-loaded lipid-core nanocapsules compared with free-olanzapine.

SIMULTANEOUS DETERMINATION OF PROTOCATECHUIC ALDEHYDE AND PROTOCATECHUIC ACID USING THE LOCALIZED SURFACE PLASMON RESONANCE PEAK OF SILVER NANOPARTICLES AND CHEMOMETRIC METHODS

A simple and sensitive spectrophotometric method is proposed for the simultaneous determination of protocatechuic acid and protocatechuic aldehyde. The method is based on the difference in the kinetic rates of the reactions of analytes with [Ag(NH3)2]+ in the presence of polyvinylpyrrolidone to produce silver nanoparticles. The data obtained were processed by chemometric methods using principal component analysis artificial neural network and partial least squares. Excellent linearity was obtained in the concentration ranges of 1.23-58.56 µg mL-1 and 0.08-30.39 µg mL-1 for PAC and PAH, respectively. The limits of detection for PAC and PAH were 0.039 and 0.025 µg mL-1, respectively.

AVALIAÇÃO DE PROPRIEDADES FÍSICAS E QUÍMICAS DE ELETRODEPÓSITOS DE Ni-W-P OBTIDOS EM CÉLULA DE HULL

Ni–W–P electrodeposits were synthesized in a Hull cell in order to simulate the obtainment under industrial conditions. Complete coverage of panels was accomplished by applying total currents of 1.0 and 2.0 A. Panels obtained with a current of 1.0 A appeared brighter. The best compositional uniformities, as determined by Energy Dispersive Spectrometer (EDS) occurred in the current density ranges of 0.6 to 3.0 A dm−2 and 1.6 to 6.0 A dm−2 obtained with 1.0 and 2.0 A, respectively. However, the best morphological characteristics, as determined by Scanning Electro Microscope (SEM), were observed in those obtained with a total current of 1.0 A. Analysis of corrosion resistance by Electrochemical Impedance Spectroscopy (EIS) and Potentiodynamic Linear Polarization (PLP) in NaCl have shown significant variations in the amount of corrosion potential, polarization resistance, and even total impedance. The alloys exhibited amorphous character (XRD) and crystallized above 400 °C to Ni and Ni3P phases, and possibly Ni–W, with a subsequent increase in hardness. The results suggest that under industrial conditions, current density variations due to the large and complex geometric shapes of substrates lead to formation of distinct alloys. Furthermore, these materials are potential substitutes for chromium deposits in many applications.

Sensitive bromatometric assay methods for finasteride in pharmaceuticals

Three sensitive spectrophotometric methods are presented for the determination of finasteride in bulk and in tablets. The methods rely on the use of bromate-bromide reagent and three dyes namely, methyl orange, indigocarmine and thymol blue as reagents. They involve the addition of a measured excess of bromate-bromide reagent to finasteride in acid medium, and after the bromination reaction is judged to be complete, the unreacted bromine is determined by reacting with a fixed amount of either methylorange and measuring the absorbance at 520 nm (method A) or indigocarmine and measuring the absorbance at 610 nm (method B) or thymol blue and measuring the absorbance at 550 nm (method C). In all the methods, the amount of insitu generated bromine reacted corresponds to the amount of finasteride. The absorbance measured at the respective wavelength is found increase linearly with the concentration of finasteride. Beer's law is obeyed in the ranges 0.25- 2.0, 0.5-6.0 and 1-12 µg mL-1 for method A, method B and method C, respectively. The calculated molar absorptivity values are 5.7x10(4), 3.12x10(4) and 1.77x10(4) L mol-1 cm-1 respectively, for method A, method B and method C, and the corresponding Sandell sensitivity values are 0.0065, 0.012 and 0.021 µg cm-2. The limits of detection (LOD) and quantification (LOQ) are also reported for all the methods. Accuracy and, intra-day and inter-day precisions of the methods were established according to the current ICH guidelines. The methods were successfully applied to the determination of finasteride in commercially available tablets and the results were found to closely agree with the label claim. The results of the methods were statistically compared with those of a reference method by applying Student's t-test and F-test. The accuracy and reliability of the methods were further confirmed by performing recovery tests via standard addition procedure.

Potentiometric and conductometric studies on the system acid-isopolytungstate and the formation of lanthanum tungstates

The stoichiometry of the polyanions formed by the action of nitric acid on sodium tungstate (< 0.01M) has been studied by means of electrometric techniques involving pH-potentiometric and conductometric titrations. The well defined inflections and breaks in the titration curves provide evidence for the existence of the polyanions, para-W12O41(10-) and meta-W12O39(6-) corresponding to the ratio of H+:WO4(2-) as 7:6 and 9:6 in the pH ranges 5.7-6.0 and 3.6-4.1, respectively. The interaction of lanthanum nitrate with sodium tungstate solutions, at specific pH levels 8.0, 5.9 and 4.0 was also studied by pH and conductometric titrations, in aqueous and alcoholic media, with each of the reagents alternatively used as titrant. The electrometric experiments provide definite evidence of the formation of normal-La2O3.3WO3, para-5La2O3.36WO3 and meta-La2O3.12WO3 tungstates in the vicinity of pH 6.3, 5.0 and 4.2, respectively. Analytical investigations on the precipitates formed confirm the results of the electrometric study.

Spectrophotometric determination of metronidazole through Schiff's base system using vanillin and PDAB reagents in pharmaceutical preparations

Two simple sensitive and reproducible spectrophotometric methods have been developed for the determination of metronidazole either in pure form or in their tablets. The proposed methods are based on the reduction of the nitro group to amino group of the drug. The reduction of metronidazole was carried out with zinc powder and 5 N hydrochloric acid at room temperature in methanol. The resulting amine was then subjected to a condensation reaction with aromatic aldehyde namely, vanillin and p-dimethyl amino benzaldehyde (PDAB) to yield yellow colored Schiff's bases. The formed Schiff's bases are quantified spectrophotometrically at their absorption maxima at 422 nm for vanillin and 494 nm for PDAB. Beer's law was obeyed in the concentration ranges 10 to 65 µg mL-1 and 5 to 40 µg mL-1 with a limit of detection (LOD) of 0.080 µg mL-1 and 0.090 µg mL-1 for vanillin and PDAB, respectively. The mean percentage recoveries were found to be 100.05 ± 0.37 and 99.01 ± 0.76 for the two methods respectively. The proposed methods were successfully applied to determine the metronidazole in their tablet formulations and the results compared favorably to that of reference methods. The proposed methods are recommended for quality control and routine analysis.

Spectrophotometric determination of ofloxacin in pharmaceuticals and human urine

Three simple and sensitive spectrophotometric methods are described for the determination of ofloxacin (OFX) in pharmaceuticals and in spiked human urine. First and second methods are based on the measurement of absorbance of OFX in 0.1 M HCl at 293 nm (method A) and 0.1 M NaOH at 287 nm, respectively. The third method is based on the measurement of 2:1 complex formed between OFX and iron(III) in H2SO4 medium, the complex peaking at 420 nm (method C). The optimum conditions for all the three methods are optimized. Beer's law is obeyed over the ranges 0.63-12.5 using method A and method B, and 10-120 µg mL-1 using method C. The apparent molar absorptivity values are calculated to be 3.5 × 10(4), 2.76 × 10(4) and 2.51 × 10³ L mol-1cm-1 for method A, method B and method C, respectively. The Sandell sensitivity, limit of detection (LOD) and limit quantification (LOQ) values are also reported. All the methods were validated in accordance with current ICH guidelines. The developed methods were employed with high degree of precision and accuracy for the estimation of total drug content in commercial tablet formulations of DOX. The results obtained from human spiked urine are satisfactory and recovery values are in the range 95.5-106.6%.

A pH optode based on thymol blue: application to determination of CO2 using flow injection analysis system

An optode based on thymol blue (TB), an acid-based indicator, has been constructed and evaluated as a detector in FIA system for CO2 determination. The dye was chemically immobilised on the surface of a bifurcated glass optical fibre bundle, using silanisation in organic media. In FIA system, hydrogen carbonate or carbonate samples are injected in a buffer carrier solution, and then are mixed with phosphoric acid solution to generate CO2, which diffuses through a PTFE membrane, in order to be collected in an acceptor carrier fluid, pumped towards to detection cell, in which the optode was adapted. The proposed system presents two linear response ranges, from 1.0 x 10-3 to 1.0 x 10-2 mol l-1, and from 2.0 x 10-2 to 0.10 mol l-1. The sampling frequency was 11 sample h-1, with good repeatability (R.S.D < 4 %, n = 10). In flow conditions the optode lifetime was 170 h. The system was applied in the analysis of commercial mineral water and the results obtained in the hydrogen carbonate determination did not differ significantly from those obtained by potentiometry, at a confidence level of 95 %.

A simple spectrophotometric method for the determination of tetracycline and doxycycline in pharmaceutical formulations using chloramine-T

A simple, rapid, accurate and inexpensive spectrophotometric method for the determination of tetracycline and doxycycline has been developed. The method is based on the reaction between these drugs and chloramine-T in alkaline medium producing red color products with absorbance maximum at the Λ = 535 and 525 nm for the tetracycline and doxycycline, respectively. The best conditions for the reactions have been found using multivariate method. Beer´s law is obeyed in a concentration ranges 1.03 x 10-5 to 3.61 x 10-4 mol L-1 and 1.75 x 10-5 to 3.48 x 10-4 mol L-1 for the tetracycline and doxycycline, respectively. The quantification limits were 5.63 x 10-6 mol L-1 and 7.12 x 10-7 mol L-1 for the tetracycline and doxycycline, respectively. The proposed method was successfully applied to the determination of these drugs in pharmaceutical formulations and the results obtained were in good agreement with those obtained by the comparative method at the 95% confidence level.

Weather based warning systems for bean angular-leaf-spot and anthracnose

Data available in the literature were used to develop a warning system for bean angular leaf spot and anthracnose, caused by Phaeoisariopsis griseola and Colletotrichum lindemuthianum, respectively. The model is based on favorable environmental conditions for the infectious process such as continuous leaf wetness duration and mean air temperature during this subphase of the pathogen-host relationship cycle. Equations published by DALLA PRIA (1977) showing the interactions of those two factors on the disease severity were used. Excell spreadsheet was used to calculate the leaf wetness period needed to cause different infection probabilities at different temperature ranges. These data were employed to elaborate critical period tables used to program a computerized electronic device that records leaf wetness duration and mean temperature and automatically shows the daily disease severity value (DDSV) for each disease. The model should be validated in field experiments under natural infection for which the daily disease severity sum (DDSS) should be identified as a criterion to indicate the beginning and the interval of fungicide applications to control both diseases.