Hidrocarbonetos policíclicos aromáticos (HPAS) em cachaça, rum, uísque e álcool combustível

The concentration of 15 polycyclic aromatic hydrocarbons (PAHs) in 57 samples of distillates (cachaça, rum, whiskey, and alcohol fuel) has been determined by HPLC-Fluorescence detection. The quantitative analytical profile of PAHs treated by Partial Least Square - Discriminant Analysis (PLS-DA) provided a good classification of the studied spirits based on their PAHs content. Additionally, the classification of the sugar cane derivatives according to the harvest practice was obtained treating the analytical data by Linear Discriminant Analysis (LDA), using naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, benz[b]fluoranthene, and benz[g,h,i]perylene, as a chemical descriptors.

Validação de metodologia para a caracterização química de bagaço de cana-de-açúcar

In this work, a methodology for the characterization of sugar cane bagasse was validated. Bagasse pre-treated with steam in a 5000 L reactor at a pressure of 15.3 kgf/cm², during 7 min, was used to test the methodology. The methodology consisted of the hydrolysis of the material with H2SO4 at 72% v/v, for the quantification of carbohydrates, organic acid, furfural and hydroxymethylfurfural by HPLC; insoluble lignin and ash by gravimetry; and soluble lignin by spectrophotometry. Linearity, repeatability, reproducibility and accuracy of the results obtained in two Research Laboratories were determined, and were considered to be suitable for the validation of the methodology.

Method validation and stability study of quercetin in topical emulsions

This study validated a high performance liquid chromatography (HPLC) method for the quantitative evaluation of quercetin in topical emulsions. The method was linear within 0.05 - 200 μg/mL range with a correlation coefficient of 0.9997, and without interference in the quercetin peak. The detection and quantitation limits were 18 and 29 ng/mL, respectively. The intra- and inter-assay precisions presented R.S.D. values lower than 2%. An average of 93% and 94% of quercetin was recovered for non-ionic and anionic emulsions, respectively. The raw material and anionic emulsion, but not non-ionic emulsion, were stable in all storage conditions for one year. The method reported is a fast and reliable HPLC technique useful for quercetin determination in topical emulsions.

Avaliação de solventes de extração por ultrassom usando-se cromatografia líquida de alta eficiência para a determinação de hidrocarbonetos policíclicos aromáticos em solos contaminados

A method using ultrasonication extraction for the determination of 17 polycyclic aromatic hydrocarbons (PAHs), selected by the USEPA and NIOSH as "consent decree" priority pollutants, in soil by High Performance Liquid Chromatography (HPLC) was studied. Separation and detection were completed in 20 min with a C18 columm, acetonitrile-water gradient elution and ultraviolet absorption and fluorescence detections. The detection limits, for a 10 µL of solution injection, were less than 9,917 ng/g in UV detection and less than 1,866 ng/g in fluorescence detection. Several organic solvents were tested for extraction of the 17 PAHs from soils. Acetone was the best solvent among the three solvents tested, and the order of the extraction efficiencies was: acetone>methanol>acetonitrile. Ultrasonication using acetone as solvent extraction was used to evaluate the biodegradation of those compounds in contaminated soil during a vermicomposting process.

Tocoferois e tocotrienois em óleos vegetais e ovos

The distribution and content of vitamin E isomers was investigated in vegetable oils and raw and cooked egg yolk in commercial restaurants. The analysis of the eight vitamin E isomers was carried out by High Performance Liquid Chromatography (HPLC) with fluorescence detection. The tocopherol and tocotrienol composition of foods varied considerably. Tocopherols were detected in greater quantity and frequency. The α-tocopherol predominated in egg yolks and olive oil while γ-tocopherol was found in high quantities in soybean and canola oils. Cooking did not cause major losses for most of the vitamin E isomers in egg yolks.

Determinação simultânea de resíduos de sulfametoxazol e trimetoprima em superfícies de equipamentos de produção

A cleaning validation method was developed and validated, based on swabbing sampling and simultaneous chromatographic determination of sulfamethoxazole (SMX) and trimethoprim (TMP) residues. The method presented limits of detection of 0.06 mg mL-1 for SMX and 0.09 mg mL-1 for TMP. It was considered selective, precise, accurate and robust according to the guidelines from ANVISA, the Brazilian regulatory agency, and International Conference on Harmonization. Mean swab recovery factors of 98.5% for SMX and 97.7% for TMP were obtained for spiked stainless steel plates. The method was successfully applied to the assay of actual swab samples collected from eleven points on an equipment surface.

Produção, purificação e aumento da performance de ciclodextrina glicosiltransferases para produção de ciclodextrinas

Biospecific affinity chromatography was used to purify three cyclodextrin glycosyl transferases (CGTases) obtained from microorganisms isolated of soil. The cyclodextrins (CDs) production by CGTases was evaluated using starches from different sources. CDs were measured through the Complexation Theory and by HPLC. CGTase from Bacillus firmus strain 7B showed the best production (30 mmol/L of β-CD and 4.3 mmol/L of γ-CD), and its cultivation conditions were optimized. The maximum enzymatic activity was achieved using lung peptone, soluble starch and agitation speed of 160 rpm. Studied CGTases were shown quite interesting for the industrial production of CDs.

Validação de métodos cromatográficos de análise: um experimento de fácil aplicação utilizando cromatografia líquida de alta eficiência (CLAE) e os princípios da "Química Verde" na determinação de metilxantinas em bebidas

The validation of analytical methods is an important step in quality control. The main objective of this study is to propose an HPLC experiment to verify the parameters of validation of chromatographic methods, based on green chemistry principles, which can be used in experimental courses of chemistry and related areas.

Efeito da acidez e de modificadores orgânicos na determinação de metilxantinas: um experimento de cromatografia liquida de alta eficiência (CLAE) empregando otimização uni e multivariada

In this work a new experiment using HPLC is proposed in order to explore the role of acidity and the organic modifiers in the determination of methylxanthines in tea and coffee. Multivariate and univariate optimizations of the experimental conditions were used.

Determinação de compostos fenólicos por cromatografia líquida de alta eficiência isocrática durante estacionamento da erva-mate

Different phenolic compound, 5- caffeoylquinic acid (5-CQA), caffeic acid (AC) and rutin (Ru) contents of yerba-mate (Ilex paraguariensis) Brazilian samples of 06 different regions of São Mateus - Paraná, during natural and accelerated industrial storage, were evaluated. For quantification, a reverse phase HPLC isocratic method was developed and validated using methanol:water (35:65 v/v) acidified with 0.5% acetic acid as mobile phase and a photodiode array detector. The six sample global average contents were (34.90 and 36.10 mg g-1) for 5-CQA, (0.18 mg g-1 and 0.23 mg g-1) for AC and (7.12 and 7.18 mg g-1) for Ru, respectively, for the natural and accelerated storage systems. The results showed that the 5-CQA and Ru content are kept constant during the storage while AC content increase only during accelerated storage.

Desenvolvimento e validação de método analítico por cromatografia líquida de alta eficiência (CLAE) para determinação de associação de ampicilinas em pó liofilizado para injeção

An analytical method has been developed and validated for the determination of an association of ampicillins in a lyophilized powder for injection by HPLC. The advantage of chromatographic method other than the microbiological one is that, it is possible to monitor precisely, out-of-specification results in quality control processes and also during stability studies, in which an association of ampicillins is present. The proposed HPLC method was developed by using forced degraded samples, in order to reach a selective analysis of ampicillins when in the presence of their degradation products. It was possible to detect benzatine and through indirect calculation, to determine the ampicillin sodium in the drug sample. The method showed to be selective, accurate, precise, robust and linear (from 45.92 to 36.04 μg mL-1 of total ampicillin and from 14.53 to 43.28 μg mL-1 of benzatine). The accuracy determined from recovery test, gave results in the range of 99.41% of total ampicillin to 100.31% of benzatine. Hence, it can be concluded that the proposed HPLC method is applicable for ampicillins determination.

Determinação simultânea de precursores de serotonina - triptofano e 5-hidroxitriptofano - em café

Epidemiological studies attributed positive effects in the central nervous system (CNS) to coffee. Among possible active constituents, serotonin, a neurotransmitter in the CNS, is present; but dietary sources do not cross the blood-brain barrier. Tryptophan and 5-hidroxytryptophan (5-HTP) are serotonin precursors and can affect brain concentrations. An ion-pair-HPLC, post-column derivatization with o-phthalaldehyde and fluorimetric detection before and after hydrolysis with NaOH and extraction with methanol:water was developed for the simultaneous determination of these compounds. It was selective, sensitive (LOD = 0.3 and 0.2 μg/mL), precise (91.3 and 94.2% recovery for tryptophan and 5-HTP, respectively), and linear from 0.3 to 40 μg/mL for both compounds. It was applied to green and roasted arabica and robusta coffees.

Determination of free urinary cortisol in cushing's syndrome using reversed-phase high performance liquid chromatography

Determination of free urinary cortisol is a test of choice in the diagnosis of Cushing's syndrome. In this study, cortisol was quantified using reversed-phase high-performance liquid chromatography (RP-HPLC) in urine samples previously extracted with ether and using triamcinolone acetonide as internal standard (IS). A BDS-Hypersil-C18® column, water-acetonitrile (72:28; v/v), with a flow rate of 1.0 mL/min and detection at 243 nm were used. This method showed to be both effective and efficient, with sensitivity and linearity ranging from 2.50 to 150 μg/L, and can be used in substitution to the radioimmunoassay technique within this concentration range.

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.