Flow injection green method for the quantitative analysis of ketoconazole in pharmaceutical preparations

A flow injection method for the quantitative analysis of ketoconazole in tablets, based on the reaction with iron (III) ions, is presented. Ketoconazole forms a red complex with iron ions in an acid medium, with maximum absorbance at 495 nm. The detection limit was estimated to be 1×10--4 mol L-1; the quantitation limit is about 3×10--4 mol L-1 and approximately 30 determinations can be performed in an hour. The results were compared with those obtained with a reference HPLC method. Statistical comparisons were done using the Student's t procedure and the F test. Complete agreement was found at the 0.95 significance level between the proposed flow injection and the HPLC procedures. The two methods present similar precision, i.e., for HPLC the mean relative standard deviation was ca. 1.2% and for FIA ca. 1.6%.

Determination of 5-aminosalicylic acid in pharmaceutical formulations by square wave voltammetry at pencil graphite electrodes

An analytical method for the determination of the anti-inflammatory drug 5-aminosalicylic acid (5-ASA) in pharmaceutical formulations using square wave voltammetry at pencil graphite electrodes was developed. After the optimization of the experimental conditions, calibration curves were obtained in the linear concentration range from 9.78 × 10-7 to 7.25 × 10-5 mol L-1 resulting in a limit of detection of 2.12 ± 0.05 x 10-8 mol L-1. Statistical tests showed that the concentrations of 5-ASA in commercial tablets and enemas obtained with the proposed voltammetric method agreed with HPLC values at a 95% confidence level.

Uso de CLAE no controle de qualidade em produtos comerciais de Nim: reprodutibilidade da ação inseticida

The Neem tree, Azadirachta indica, provides many useful compounds that are used as pesticides. However, the efficiency in field of products like neem oil can be committed because they have not been observed reproductive content of secondary metabolic like azadirachtin. Based on reverse-phase high-performance liquid chromatography (HPLC) a new method was developed to permit the rapid quantitative analysis of azadirachtin from seeds, extracts and oil of Neem. In the present study it was evaluated the azadirachtin quantitative variation among various Neem's extracts and seeds showing the importance of quality control for reproduction of the insecticide efficiency, using S. frugiperda as target insect.

Degradação eletroquímica do cloranfenicol em reator de fluxo

This paper reports a study of electrochemical degradation of the chloramphenicol antibiotic in aqueous medium using a flow-by reactor with DSA® anode. The process efficiency was monitored by chloramphenicol concentration analysis with liquid chromatography (HPLC) during the experiments. Analysis of Total Organic Carbon (TOC) was performed to estimate the degradation degree and Ion Chromatography (IC) was performed to determinate inorganic ions formed during the eletrochemical degradation process. In electrochemical flow-by reactor, 52% of chloramphenicol was degraded, with 12% TOC reduction. IC analysis showed the production of chloride ions (25 mg L-1), nitrate ions (6 mg L-1) and nitrite ions (4.5 mg L-1).

Development and validation of a LC-method for the determination of phenols in a pharmaceutical formulation containing extracts from Stryphnodendron adstringens

A sensitive RP-HPLC method with UV detection successfully measured phenol(s) in an ointment containing 3% Stryphnodendron adstringens extract. Chromatography used acetonitrile (0.05% trifluoroacetic acid):water (0.05% trifluoroacetic acid) (v/v), flow rate 0.8 mL min-1. Quantitation was accomplished by the external-standard method. Linearity for 2.00 to 16.00 μg mL-1 (gallic acid) and 1.14 to 18.24 μg mL-1 (gallocatechin) was established. Intra- and inter-day precision levels were under 5%. LOD and LOQ were 0.231 and 0.770 μg mL-1 (gallic acid) and 0.151 and 0.504 μg mL-1 (gallocatechin), respectively. Determination of phenols was unaffected by product excipients.

Otimização e validação de método para determinação de ácidos orgânicos em vinhos por cromatografia líquida de alta eficiência

The organic acids (tartaric, malic, citric, lactic and succinic) are de main components responsible for the acidity in the wine. This method for simultaneous determination of organic acids and interfering peaks in wines can be achieved in 16 min. The sample preceded by a dilution and filtration step. The chromatographic separation required one reversed phase column, isocratic mobile phase (acetonitrila, formic acid in water) and detection wavelength was set at 212 nm. The validation confirmed good repeatability, recovery and application in red and white wines.

Synchronous scanning phosphorimetry for the selective determination of chrysene: a metrological study

Room-temperature phosphorimetry was used to quantify trace levels of chrysene in sugar-cane spirits and in fish bile. A selective phosphorescence enhancer (AgNO3) and synchronous scanning allowed the detection of ng amounts of chrysene. Accuracy (113 ± 17%) and selectivity was evaluated using the CRM-NIST-1647d - Priority Pollutant Polycyclic Aromatic Hydrocarbons in acetonitrile. Analysis of sugar-cane spirit samples enabled recovery of 108 ± 18% which agreed with the one achieved using HPLC. Method's uncertainty was equivalent to 3.4 ng of the analyte, however, the analyte pre-concentration (SPE) improved sensibility and minimized the relative uncertainty. Characterization and homogeneity studies in fish bile were also performed.

Avaliação do uso de inibidores de etileno sobre a produção de compostos voláteis e de mangiferina em manga

Effects of two ethylene inhibitors, 1-methylcylopropene (1-MCP) and aminoethoxyvinylglycine (AVG), on production of volatile compounds and mangiferin (a bioactive xanthone) in 'Tommy Atkins' mango fruit were investigated. Volatile composition and mangiferin content, in treated and untreated fruits at three maturity, stages were determined by SPME-GC-MS and HPLC, respectively. These chromatographical analysis revealed that the volatile profiles and mangiferin concentrations were not significantly different, suggesting that the use of ethylene inhibitors does not affect the mango aroma and functional properties relative to this xanthone. Moreover, a simple, precise and accurate HPLC method was developed for quantifying mangiferin in mango pulp.

Fases estacionárias modernas para cromatografia líquida de alta eficiência em fase reversa

This review first discusses the limitations of many of the supports and stationary phases used in reversed phase high performance liquid chromatography and then describes those, developed more recently, that present better stabilities and more versatile selectivities. Emphases will be given to stationary phases that use higher purity silicas, hybrid silicas, monolithic silicas, metallic oxides and mixed oxides as supports and those that have embedded polar groups or contain phenyl or fluoro groups as the stationary phase as well as the phases used for mixed mode or hydrophilic interaction separations. These modern stationary phases facilitate the analysis of complex mixtures.

Análise comparativa entre vários métodos de quantificação de hemiceluloses da madeira de eucalipto

Pulp hemicelluloses can be extracted with NaOH and quantified by colorimetric and gravimetric techniques. However the most usual methods to measure eucalyptus pulp hemicelluloses have been through the pentosan method or through xylan analyses by GC or HPLC techniques. In this study a comparison was made between the more traditional methods and indirect method of NaOH 5% extraction followed by colorimetric analyses. It was observed that the content of NaOH 5% extract correlates very well with pulp xylan content and reasonably well with the pentosan content. It is concluded that the 5% NaOH solubility method can be used in replacement of the other two, since it is faster, simpler and less costly to carry out than the others.

Validação de método para a determinação de 5-hidroximetilfurfural em mel por cromatografia líquida e sua influência na qualidade do produto

In honey 5-hydroxymethyl-2-furaldehyde (HMF) is one of the most typical products of degradation: it is usually absent in fresh honey, but its concentration tends to rise as a result of heating processes or long-term storage. The validation protocol was performed in terms of detection and quantification limits, precision (by repeatability and intermediate precision), linearity and accuracy (by recovery tests). The method has been tested on 15 honey samples of different ages and geographical origin. HMF correlated highly with the age of the samples has been considered a very important parameter to put these honeys on the market or not and/or to estimate their shelf life.

Validación de un método analítico empleando cromatografía líquida de alta eficiencia para la determinación de ibuprofeno en medios biorrelevantes

An analytical method by liquid chromatography has been proposed and validated to study the apparent solubility of ibuprofen in biorelevant dissolution media. The main properties of the studied media were pH values of 5.0 and 6.5 and the presence or absence of some natural surfactant agents. The parameters evaluated were specificity, linearity, precision, accuracy, and detection and quantification limits, as well as the drug stability under the analysis conditions. The developed method was useful to determine the apparent solubility of this drug as a function of temperature and surfactants concentration to demonstrate the validity of the Biopharmaceutics Classification System.

Determinação de hormônios estrógenos em água potável usando CLAE-DAD

An analytical procedure for determination of estriol, 17β-estradiol, estrone and 17α-ethinylestradiol in drinking water is presented. The method employs solid phase extraction (SPE) and sample dechlorination as cleanup procedures, followed by HPLC-DAD analysis. Validation was carried out using RE No. 899/2003 guidelines established by the Agência Nacional de Vigilância Sanitária (National Agency of Sanitary Surveillance, Brazil), with some adaptations. The statistically evaluated results have shown that the method is selective, precise (0,06% to 19,40% CV) and accurate (91,52% to 109,41% average recoveries). The developed method was applied to the analysis of these contaminants in drinking water from São Luís, MA.

Desenvolvimento de método analítico para quantificação do efavirenz por espectrofotometria no UV-Vis

An UV-Vis spectrophotometry analytical method for quantifying Efavirenz was developed and validated as an alternative to replace the HPLC current method. The report method presents sample concentration of 10 μg mL-1, dissolved in a solution ethanol:water (60:40, v/v), economic and technically adequate for the purpose adopted. The results and the statistical treated proved that the method being considered an precise and accurate analytical low cost alternative for laboratory routine. The adaptability of this method in product and other analytical methods development has been challenged by mathematical calculation of drug extinction coefficient in water and methanol and practical experiments, showing interesting results.

Benzo(a)pireno, carbamato de etila e metanol em cachaças

The objective of this work was to evaluate the presence of benzo(a)pyrene (BaP), ethyl carbamate (EC) and methanol in 61 samples of cachaça. The quantification of BaP was carried out using HPLC with fluorescence detection, EC concentrations was determined by GC/MS and that of methanol, by GC/FID. In all samples, the concentration of methanol remained below 5 mg 100 mL-1 absolute alcohol. The results of BaP varied from <0.03 to 0.86 μg L-1; the values of EC exceeded the limit established by Brazilian legislation (150 μg L-1) in 53% of the samples.