Método colorimétrico para determinação de dióxido de nitrogênio atmosférico com preconcentração em coluna de c-18

An alternative analytical method for nitrogen dioxide (NO2) in atmosphere was developed. The collection of NO2 is performed by a Sep-Pack C-18 cartridge impregnated with 11% (v/v) of triethanolamine plus 3,6 % (v/v) of ethylene glycol plus 25 % (v/v) of acetone combined solution. When the impregnating is used, NO2 is collected with good repeatibility (CV = 3,3 %). The NO2 absorbed in the sampler was stripped from the sorbent with a methanol 5% (v/v) aqueous solution and was determined by colorimetry as nitrite by using the Griess-Saltzman reagent. The detection limit of 1,4 ppb for 60 min sampling at 0,5 L min-1 flow rate was obtained. Preparation and conditioning procedures for TEA-C-18 cartridge, sampling flow rate, absorption capacity and interference of other species are discussed.

Determinação de alfa-Tocoferol em alho irradiado utilizando cromatografia líquida de alta eficiência (CLAE)

The effects of 60Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the alpha-tocopherol concentration were studied. The alpha-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The alpha-tocopherol was determined through normal-phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic alpha-tocopherol content.

Determinação enzimática de dopamina em formulações farmacêuticas utilizando sistema de análise por injeção em fluxo com extrato bruto de abacate (Persea americana)

In this work, a spectrophotometric flow injection analysis system using a crude extract of avocado (Persea americana) as a source of polyphenol oxidase to dopamine determination was developed. The substrates and enzyme concentrations from 2.4x10-7 to 5.3x10-4 mol L-1 and 28 to 332 units mL-1 were evaluated, respectively. In addition, the FIA parameters such as sample loop (50 to 500 µL), flow rate (1.4 to 4.3 mL min-1) and reactor length (100 to 500 cm) were also evaluated in a 0.1 mol L-1 phosphate buffer solution (pH 7.0). Dopamine solution concentrations were determined using 277 units mL-1 enzyme solution, 400 mL enzyme loop, 375 µL sample loop, 2.2 mL min-1 flow rate and a reactor of 350 cm. The analytical curve showed a linearity from 5.3x10-5 to 5.3x10-4 mol L-1 dopamine with a detection limit of 1.3x10-5 mol L-1. The analytical frequency was 46 h-1 and the RSD lower than 0.5% for 5.3x10-4 mol L-1 dopamine solution (n=10). A paired t-test showed that all results obtained for dopamine in commercial formulations using the proposed flow injection procedure and a spectrophotometric procedure agree at the 95% confidence level.

Determinação potenciométrica em fluxo de cloreto de cetilpiridinio em desinfectantes bucais

The work describes a new procedure for cetylpyridinium chloride determination in oral disinfectants, based on a flow-injection system with potentiometric detection. The determination was based on the measurement of picrate concentration decrease as result of ion-pair reaction with the analyte present in the injected sample. In the optimised set-up the sample injection volume was kept at 400 µL and merged downstream with the reagent solution containing 1,0 x10-5 mol/L of picrate adjusted to pH 5.0 with citrate/citric acid buffer. The flow rate was fixed at 8 mL/min and the reactor length at 40 cm. The proposed procedure enables the determination of cetylpyridinium in the analytical range of 5,0x10-6 - 7,5x10-5 mol/L at a sampling rate of 60/h. The results for real samples had a precision better than 3% and were comparable to the labelled values.

Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Análise de ácidos graxos não-esterificados de plasma humano por cromatografia gasosa capilar com injeção sem divisão de fluxo

The aim of the present work was to test the combination of non-esterified fatty acid (NEFA) isolation using fumed silicon dioxide with capillary gas-chromatography (C-GC) with splitless injection for the analysis of NEFAs in human plasma. Injection volume, solvent re-condensation and split purge flow-rate were the parameters evaluated for the analysis of fatty acid methyl esters by C-GC. The use of a solvent re-condensation technique, associated with 1.0 µL injection and a split purge flow rate of 80 mL/min resulted in satisfactory analysis of NEFAs. Fourteen fatty acids were identified in plasma samples, ranging from 2.03 to 184.0 µmol/L. The combination of both techniques proved useful for routine analyses of plasma NEFAs.

A novel method for fast enrichment and monitoring of hexavalent and trivalent chromium at the ppt level with modified silica MCM-41 and its determination by inductively coupled plasma optical emission spectrometry

Chromium(III) at the ng L-1 level was extracted using partially silylated MCM-41 modified by a tetraazamacrocyclic compound (TAMC) and determined by inductively coupled plasma optical emision spectrometry (ICP OES). The extraction time and efficiency, pH and flow rate, type and minimum amount of stripping acid, and break- through volume were investigated. The method's enrichment factor and detection limit are 300 and 45.5 pg mL-1, respectively. The maximum capacity of the 10 mg of modified silylated MCM-41 was found to be 400.5±4.7 µg for Cr(III). The method was applied to the determination of Cr(III) and Cr(VI) in the wastewater of the chromium electroplating industry and in environmental and biological samples (black tea, hot and black pepper).

Uso da pressão gerada por uma coluna de água para controle da vazão em sistemas de análises em fluxo

This work presents a new approach to control the flow rate in hydrodynamic flow experiments. The combination of air pressure generated by an aquarium air pump and the pressure generated by a water column were used for this purpose. This device supports a stable flow rate without pulsation for a long period of time. Furthermore, the flow rate can be easily controlled at various values in one or more streams. The performance of this approach was investigated using Fe(CN)6(4-) solutions in flowing systems using amperometric and voltammetric detection in wall-jet configuration. The results showed that the performance of the proposed device was better than a commercial peristaltic pump. It suggests that this approach can be used successfully in flow analysis systems.

Determination of etoricoxib in human plasma using automated on-line solid-phase extraction coupled with LC-APCI/MS/MS

A liquid chromatography-tandem mass spectrometry method with atmospheric pressure chemical ionization (LC-APCI/MS/MS) was validated for the determination of etoricoxib in human plasma using antipyrin as internal standard, followed by on-line solid-phase extraction. The method was performed on a Luna C18 column and the mobile phase consisted of acetonitrile:water (95:5, v/v)/ammonium acetate (pH 4.0; 10 mM), run at a flow rate of 0.6 mL/min. The method was linear in the range of 1-5000 ng/mL (r²>0.99). The lower limit of quantitation was 1 ng/mL. The recoveries were within 93.72-96.18%. Moreover, method validation demonstrated acceptable results for the precision, accuracy and stability studies.

Estudo da degradação de ranitidina via H2O2 eletrogerado/Fenton em um reator eletroquímico com eletrodos de difusão gasosa

The study of the electrochemical degradation of the ranitidine was developed using an electrochemical reactor with a gas diffusion electrode (GDE) as cathode. The electrolysis experiments was performed at constant current (1 < A < 10) and flow rate of 200 L h-1. The process of drug degradation, chemical/electrochemical and electro-Fenton ways, using electrochemical reactor showed best efficiency at current values of > 4 A. The process reached a production of 630 mg L-1 of the H2O2 at 7 A. The ranitidine concentrations was reduced in 99.9% (HPLC) and chemical oxygen demand (COD) was reduced in 86.7% by electro-Fenton.

Desenvolvimento e validação de um método analítico rápido por cromatografia líquida de alta eficiência para determinação de nimesulida em estudos de liberação in vitro

A high performance liquid chromatography (HPLC) method has been developed for a rapid determination of nimesulide in dissolution studies. Nimesulide was analyzed using 5 µm Lichrospher® RP-18 column (125 x 4 mm i.d.) and mobile phase acetonitrile: phosphate buffer pH=6.0 (55:45) at a flow-rate of 1.0 mL min-1. Detection was carried out at 300 nm at 25 ºC. The method was applied to analysis of nimesulide in in vitro release studies and showed a rapid and efficient analytical alternative for evaluation of dissolution profile of nimesulide.

Removal of phenol and conventional pollutants from aqueous effluent by chitosan and chitin

The present study deals with phenol adsorption on chitin and chitosan and removal of contaminants from wastewater of a petroleum refinery. The adsorption kinetic data were best fitted to first- and second-order models for chitosan and chitin, respectively. The results of adsorption isotherms showed Langmuir model more appropriately described than a Freundlich model for both adsorbents. The adsorption capacity was 1.96 and 1.26 mg/g for chitin and chitosan, respectively. Maximum removal of phenol was about 70-80% (flow rate: 1.5 mL/min, bed height: 18.5 cm, and 30 mg/L of phenol. Wastewater treatment with chitin in a fixed-bed system showed reductions of about 52 and 92% for COD and oil and greases, and for chitosan 65 and 67%, respectively. The results show improvement of the effluent quality after treatment with chitin and chitosan.

Determination of phenobarbital in human plasma by a specific liquid chromatography method: application to a bioequivalence study

A liquid chromatography method was developed and validated for the determination of phenobarbital in human plasma using phenytoin as internal standard. The drugs were extracted from plasma by liquid-liquid extraction and separated isocratically on a C12 analytical column, maintained at 35 ºC, with water:acetonitrile:methanol (58.8:15.2:26, v/v/v) as mobile phase, run at a flow rate of 1.2 mL/min with detection at 205 nm. The method was linear in the range of 0.1-4 μg/mL (r²=0.9999) and demonstrated acceptable results for the precision, accuracy and stability studies. The method was successfully applied for the bioequivalence study of two tablet formulations (test and reference) of phenobarbital 100 mg after single oral dose administration to healthy human volunteers.

Determinação de citrato de sildenafila e de tadalafila por cromatografia líquida de ultraeficiência com detecção por arranjo de diodos (CLUE-DAD)

A simple ultra-performance liquid chromatographic method for the simultaneous determination of sildenafil citrate and tadalafil was developed and validated. Sample preparation was dissolution in methanol, followed by centrifugation and dilution (1:10) with methanol. Analysis was performed in an Acquity® UPLC system with Acquity® BEH C18 column (2.1 x 50 mm, with 1.7 μm particles). The elution was isocratic with phosphate buffer pH 2.3 and acetonitrile (65:35, v/v) at a flow rate of 0.7 mL/min. The method presented adequate specificity, linearity, precision and accuracy and allowed the determination of the drugs in seized forensic samples.

Estudo da eficiência de degradação de tetracloreto de carbono por plasma térmico e caracterização dos produtos formados

Decomposition of carbon tetrachloride in a DC thermal plasma reactor was investigated in argon atmosphere. The operational parameters such as plasma torch power and argon flow rate versus CCl4 conversion were examined. The CCl4 net degradation was determined by GC-FID, the chlorine produced was quantified by iodometric titration, the solid carbon was characterised by Raman spectroscopy and by BET analysis. The solid carbon collected inside de plasma reactor was submitted to solid/liquid extraction and the desorbed species were identified by GC-MS.