Cromatografia gasosa ultrarrápida: uma visão geral sobre parâmetros, instrumentação e aplicações

Since the introduction of GC there has been an ongoing interest in reducing time of analysis resulting in new terms and definitions such as ultra fast gas chromatography (UF-GC). One of the most used definitions describes UF-GC as a technique that combines the employment of short narrow bore column with very fast temperature programming rates producing chromatographic peaks in the range of 50 ms and allowing separations times in 1-2 min or less. This paper summarizes the analytical approaches, the main parameters involved and the instrumentation towards UF-GC.

Development and validation of a stability-indicating UPLC method for rosuvastatin and its related impurities in pharmaceutical dosage forms

The present work describes a novel stability-indicating reversed-phase ultra performance liquid chromatography method for the separation and quantification of rosuvastatin (RSV) and its related impurities in the pharmaceutical dosage forms under forced degradation conditions. An unknown degradation impurity detected in the acid degradation was identified by using quadrupole time-of-flight mass spectrometry. The chromatographic separation was carried out on C-18 column (100 x 2.1 mm, 1.7 μm) using isocratic elution with methanol and 0.1% trifluoroacetic acid (50:50). The total run time was 12 min within which RSV as well as all related impurities and degradation products were separated. The developed method was validated for RSV and related impurities in pharmaceutical dosage forms.

Caracterização espectroscópica multivariada do potencial antioxidante de vinhos

In this work the antioxidant capacity of red wine samples was characterized by conventional spectroscopic and chromatographic methodologies, regarding chemical parameters like color, total polyphenolic and resveratrol content, and antioxidant activity. Additionally, multivariate calibration models were developed to predict the antioxidant activity, using partial least square regression and the spectral data registered between 400 and 800 nm. Even when a close correlation between the evaluated parameters has been expected many inconsistencies were observed, probably on account of the low selectivity of the conventional methodologies. Models developed from mean-centered spectra and using 4 latent variables allowed high prevision capacity of the antioxidant activity, permitting relative errors lower than 3%.

Aumento da resposta analítica por meio da otimização do sistema de injeção sem divisão de fluxo em cromatografia gasosa empregando a lei dos gases ideais

This paper reports the development of an easy, fast and effective procedure for the verification of the ideal gas law in splitless injection systems in order to improve the response. Results of a group of pesticides were used to demonstrate the suitability of the approach. The procedure helps establish experimental parameters through theoretical aspects. The improved instrumental response allowed extraction with lower sample volumes, the minimization of time and costs and the simplification of sample preparation.

Aplicação de quitosana como suporte para a imobilização de enzimas de interesse industrial

Chitosan, poly[β-(1-4)-linked-2-amino-2-deoxy-D-glucose], is the N-deacetylated product of chitin which is a major component of arthropod and crustacean shells such as lobsters, crabs, shrimps, and cuttlefishes. In addition, chitosan has many significant biological and chemical properties such as biodegradability, biocompatibility and bioactivity as well as polycationic properties. Thus, it has been widely used in many industrial and biomedical applications including wastewater treatment, chromatographic support, carriers for controlled drug delivery and enzyme immobilization. This review is an insight into the exploitation of utilization of chitosan based-supports in different geometrical configurations on the immobilization of enzymes by different protocols for further application in biotransformation reactions.

Determinação rápida de oseltamivir em cápsulas por cromatografia líquida de ultraeficiência com detector por arranjo de diodos

A simple and rapid ultra-performance liquid chromatographic method for determination of oseltamivir in capsules was developed and validated. The mobile phase consisted of 5 mmol/L triethylammonium buffer (pH 3.0) and acetonitrile (70:30, v/v). Separation was performed in a Hypersil Gold® column, with octylsilil as stationary phase (100 x 2.1 mm, p.d. 1.9 µm). Chromatography run time was 1.2 min. The method presented adequate specificity, linearity, precision, ruggedness and accuracy and was adequate for determination of oseltamivir in capsules.

Avaliação do perfil de dissolução de medicamentos utilizando-se espectroscopia eletrônica multivariada

In this work the evaluation of the dissolution profile of captopril-hydrochlorothiazide and zidovudine-lamivudine associations were carried out by multivariate spectroscopic method. The models were developed by partial least square regression from 20 synthetic mixtures using mean-centered spectral data. The external validation was accomplished with 5 synthetic mixtures shown mean prevision error of about 1%. Good agreement was observed in the analyses of commercial drugs (content uniformity and dissolution profile), considering the results obtained by the standard chromatographic method, with prevision error lower than 10%.

Validação de método multirresíduo para determinação de pesticidas em alimentos empregando QuEChERS E UPLC-MS/MS

This paper presents a practical and rapid method which was validated for simultaneous quantification and confirmation of 29 pesticides in fruits and vegetables using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted following the method known as QuEChERS. Using the developed chromatographic conditions, the pesticides can be separated in less than 9 min. Two multiple reaction monitoring (MRM) assays were used for each pesticide. Four representative matrices (lettuce, tomato, apple and grapes) were selected to investigate the effect in recoveries and precision. Typical recoveries ranged from 70-120%, with relative standard deviation (RSDs) lower than 20%.

Investigando cinza da casca do arroz como fase estacionária em cromatografia: uma proposta de aula experimental nos cursos de graduação

This article describes an experiment that involves the extraction and separation of the pigments of spinach extract by column chromatography using the silica obtained from rice husk ash as a stationary phase. The experimental procedure is very simple to apply in the chemistry laboratory, and allowed to illustrate some concepts of organic chemistry: structure of organic molecules, solubility, polarity, extraction, partition coefficient, adsorption and retention factor (Rf), as well as objectives and fundamentals of chromatographic methods. The experiment can be carried out in a 4 h period.

Performance characteristics of high performance liquid chromatography, first order derivative UV spectrophotometry and bioassay for fluconazole determination in capsules

The bioassay, first order derivative UV spectrophotometry and chromatographic methods for assaying fluconazole capsules were compared. They have shown great advantages over the earlier published methods. Using the first order derivative, the UV spectrophotometry method does not suffer interference of excipients. Validation parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation were determined. All methods were linear and reliable within acceptable limits for antibiotic pharmaceutical preparations being accurate, precise and reproducible. The application of each method as a routine analysis should be investigated considering cost, simplicity, equipment, solvents, speed, and application to large or small workloads.

Identificação de extratos etanólicos de madeiras utilizando seu espectro eletrônico de absorção e análise multivariada

The application of multivariate analysis to spectrophotometric (UV) data was explored for distinguishing extracts of cachaça woods commonly used in the manufacture of casks for aging cachaças (oak, cabreúva-parda, jatobá, amendoim and canela-sassafrás). Absorbances close to 280 nm were more strongly correlated with oak and jatobá woods, whereas absorbances near 230 nm were more correlated with canela-sassafrás and cabreúva-parda. A comparison between the spectrophotometric model and the model based on chromatographic (HPLC-DAD) data was carried out. The spectrophotometric model better explained the variance data (PC1 + PC2 = 91%) exhibiting potential as a routine method for checking aged spirits.

Desenvolvimento e validação de método analítico por CLAE para a quantificação simultânea de dipropionato de betametasona e fosfato sódico de betametasona em suspensão injetável

A reversed-phase HPLC method was developed and validated to separate and simultaneously quantify the association of betamethasone sodium phosphate (BP) and betamethasone dipropionate (BD) in injectable suspensions. Chromatographic conditions were ternary gradient elution at 1.6 mL/min on a C18 column with 254 nm. The linearity of the method was established in the range 120 to 280 mg/mL BD, and 48 to 112 mg/mL BP. The RSD of intermediate precision of the method was <1% and recoveries were 99-101% for both drugs. The method proved selective, linear, precise, accurate and robust for quantifying BP and BD in commercial injectable suspensions.

Set-up of a method using LC-UV to assay mometasone furoate in pharmaceutical dosage forms

A reliable method using LC-UV to assay mometasone furoate (MF) in creams or nasal sprays using the same chromatographic conditions was set up. Methanol:water 80:20 (v/v) (1.0 mL min-1) was used as mobile phase. MF was detected at 248 nm and analyzed in a concentration range from 1.0 to 20.0 µg mL-1. The method provided acceptable theoretical plates, peak simmetry, peak tailing factor and peak resolution a short run (5 min). The method showed specificity, good linearity (r = 0.9999) and the quantification limit was 0.379 µg mL-1. Furthermore, the method was precise (RSD < 2.0%), accurate (recovery > 97%) and robust.

Development and validation of a novel stability indicating RP-UPLC method for simultaneous determination of nizatidine, methylparaben and propylparaben in oral liquid pharmaceutical formulation

A selective and accurate stability-indicating gradient reverse phase ultra performance liquid chromatographic method has been developed and validated for the simultaneous determination of nizatidine, methylparaben and propylparaben in pharmaceutical oral liquid formulation. The separation was achieved on Acquity UPLC TM HSS T3 1.8 µm column by using mobile phase containing a gradient mixture of solvent A (0.02 Mol L-1 KH2PO4, pH 7.5) and B (60:40 v/v mixture of methanol and acetonitrile) at flow rate of 0.4 mL min-1. Drug product was exposed to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

Specificity and selectivity improvement in doping analysis using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry

Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry was used for the identification of forty doping agents. The improvement in the specificity was remarkable, allowing the resolution of analytes that could not be done by one-dimensional chromatographic systems. The sensitivity observed for different classes of prohibited substances was clearly below the value required by the World Anti-Doping Agency. In addition time-of-flight mass spectrometry gives full spectrum for all analytes without any interference from the matrix, resulting in selectivity improvements. These results could support the implementation of an exhaustive monitoring approach for hundreds of doping agents in a single injection.