Validação de metodologia analítica para o doseamento simultâneo de mebendazol e tiabendazol por cromatografia líquida de alta eficiência

The aim of this work was to develop and validate an analytical methodology for simultaneous determination of mebendazole and thiabendazole, two benzimidazoles used as anthelmintics. The method was based on high performance liquid chromatography, using a C18 column, a mobile phase composed of KH2PO4 0.05 mol L-1 and methanol 40:60 (v/v) and UV detection at 312 nm. The results showed that the method presented linearity from 60.0 to 140.0 µg mL-1 for mebendazole and from 99.6 to 232.4 g µL-1 for thiabendazole and it was considered selective, accurate, precise and robust according to the specific resolution from ANVISA, the Brazilian regulatory agency.

Dessorção iônica e degradação de filmes de polipirrol dopado com dodecilsulfato induzidas por elétrons de alta energia

Electron stimulated ion desorption (ESID) and degradation studies of polypyrrole doped with dodecylsulfate (PPy/DS) deposited on FTO were performed using time-of-flight mass spectrometry (TOF-MS) for ion analysis. The results suggest a strong contribution from fragments of the dodecylsulfate hydrocarbon chain to the mass spectra. In the 650-1500 eV energy range the ion yield curves show maxima at about 600, 1200 and 1400 eV, which can be related to carbon, nitrogen and oxygen-containing fragments, respectively, and interpreted in terms of the Auger Stimulated Ion Desorption (ASID) mechanism. Degradation studies indicate rapid loss of heavier hydrocarbons and an increase of bulk and substrate fragments. Some degradation profiles suggest formation of new species.

Determinação da espessura da camada polimérica de fases estacionárias imobilizadas para cromatografia líquida de alta eficiência por termogravimetria

This paper presents a simple and practical thermogravimetric method for determining the layer thickness of immobilized polymer stationary phases used in reversed-phase high-performance liquid chromatography. In this method, the weight loss of different polysiloxanes immobilized onto chromatographic supports, determined over the temperature range 150-650 ºC, demonstrated excellent agreement with the sum of carbon and hydrogen content obtained by elemental analysis. The results presented here suggest that the thermogravimetric procedure is an accurate and precise method to determine the polymeric material content on polymer-coated stationary phases.

Composição química dos óleos essenciais das folhas de seis espécies do gênero Baccharis de "Campos de Altitude" da mata atlântica paulista

The essential oils from the leaves of six species of the Baccharis genus (B. dracunculifolia, B. microdonta, B. regnelli, B. schultzii, B. trimera, and B. uncinella), collected in the "Campos de Altitude" of the Atlantic Forest (SP), were extracted using hydrodistillation procedures and analyzed by GC and GC/MS. There was a predominance of sesquiterpenes in all studied oils as b-elemene in B. dracunculifolia and B. regnelli, a-humulene in B. trimera, g-gurjunene in B. schultzii, bicyclogermacrene in B. regnelli, d-cadinene in B. regnelli and B. uncinella, spathulenol in B. schultzii, caryophyllene oxide in B. microdonta and guaiol in B. uncinella. However, a high amount of monoterpenes was also observed in B. uncinella (a-pinene), B. regnelli (d-car-3-ene) and B. schultzii (limonene). The chemical compounds of the essential oils of B. schultzii, B. regnelli and B. microdonta are described for the first time in this work.

Nanocompósitos cerâmicos a partir do processo de moagem mecânica de alta energia

Pb/Ti, Sn and Mg-based nanocomposite materials were prepared by the high-energy mechanical milling of commercial powders. The surface of these ceramic compounds was strongly influenced by the doping, diameter of the milling spheres and time of the mechanical milling (amorphization process). Such milling leads to the formation of nanocrystalline materials. The mechanical processing parameters of these compounds were investigated through Brunauer, Emmett and Teller isotherms, wide angle X-ray diffraction, transmission electron microscopy and CO2 adsorption.

Desenvolvimento e validação de método analítico para determinação simultânea de lamivudina, zidovudina e nevirapina em comprimidos dose-fixa combinada por cromatografia líquida de alta eficiência

An analytical method has been developed and validated for the quantitation of lamivudine, zidovudine and nevirapine in the fixed-dose combination film-coated tablet by high performance liquid chromatography, in accordance with RE No. 899/2003, National Sanitary Surveillance Agency. It was based on an isocratic elution system with a potassium phosphate buffer pH 3.0: acetonitrile (60:40 v/v) mobile phase, C18, 250 x 46 mm column, 10µm particle size, λ 270 nm. The statistically evaluated results have shown that the method is specific, precise, accurate, and robust, ensuring the analytical safety of 3TC, AZT and NVP determination, which emerges as a new therapeutic alternative for antiretroviral treatment.

Quantificação simultânea de indicadores biológicos de exposição a solventes orgânicos por cromatografia líquida de alta eficiência

Biological monitoring is very important to guarantee health to workers. This method was developed for simultaneous determination of xylene, toluene, styrene and ethylbenzene metabolites. It involves only dilution and centrifugation of urine samples and improved chromatographic conditions. Analyses show recovery > 95%; r² > 0.99; intermediate precision CV% < 6% and % bias < ±10. Exposed subjects presented at least three metabolites in urine. The method proved to be feasible, reliable and important in biological monitoring, especially in exposure to organic solvent mixtures.

Otimização de método para determinação de flavonóis e flavonas em frutas por cromatografia líquida de alta eficiência utilizando delineamento estatístico e análise de superfície de resposta

This work optimized the HPLC conditions for the simultaneous determination of luteolin, apigenin, myricetin, quercetin and kaempferol in aglycone form, as well defined the best conditions for hydrolysis/extraction of these flavonoids in fruits, using the statistical central composite design and response surface analysis. A reverse phase method was developed using a gradient of methanol/water acidified with 0.3% formic acid as mobile phase and a photodiode array detector. The samples were extracted with methanol/water (50:50 v/v) at 90 ºC. The optimum time and HCl concentration varied for the different fruits investigated, demonstrating the necessity of optimizing these conditions for each fruit analyzed. Good recovery (87.1 to 96.3%), repeatability and linearity were obtained.

Desenvolvimento e validação de método por cromatografia líquida de alta eficiência para determinação simultânea das impurezas timina e timidina na matéria-prima estavudina

A HPLC method was developed to quantify thymine and thymidine impurities in stavudine bulk drug. The separation was carried out in isocratic mode using methanol/water (20:80) as mobile phase, a C18 column and UV detection at 266 nm. The method provided selectivity based on peak purities and resolution among peaks. It was linear over the range of 0.5-5.0 µg/mL. The quantitation limits were 0.021 µg/mL for thymine and 0.134 µg/mL for thymidine. The average accuracies of three concentrations ranged from 97.06 to 102.61% and precision was close to 1%. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.

Determinação simultânea de creatinina e indicadores biológicos de exposição ao tolueno, estireno e xilenos em urina por cromatografia líquida de alta eficiência

A simple liquid chromatographic method for the simultaneous determination of creatinine, hippuric acid, mandelic acid, phenylglyoxylic acid and o, m and p-methylhippuric acids was developed and validated. Sample preparation was only dilution with water (1:10), followed by centrifugation. Analysis was performed in a reversed phase column (Lichrospher RP 8ec), 250 x 4.0 mm, with isocratic elution with phosphate buffer pH 2.3 and acetonitrile (90:10, v/v). The method presents adequate linearity, precision and accuracy and allows the simultaneous determination of the biomarkers of exposure to toluene, xylene and styrene together with creatinine, reducing cost and laboratory time.

Validação de metodologia analítica por cromatografia líquida de alta eficiência para quantificação de bupivacaína (S75-R25) em nanoesferas de poli(lactídeo-co-glicolídeo)

Bupivacaine (S75-R25, NovaBupi®) is an amide type local anesthetic widely used. The present work consists of the development and validation of analytical methodology for evaluation of NovaBupi® content in the poly-lactide-co-glycolide nanospheres (PLGA-NS) by high performance liquid chromatography. The separation was made using the reversed-phase column LC-18, acetonitrile/phosphate buffer 85:15 v/v as mobile phase and detection at 220 nm. The results obtained show that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 10-220.0 g/mL of NovaBupi®. The method was applied to determine the encapsulation efficiency and evaluate the release profile of NovaBupi®, showing good results.

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.

Determinação de 3,4-metilenodioximetanfetamina (MDMA) em comprimidos de Ecstasy por cromatografia líquida de alta eficiência com detecção por fluorescência (CLAE-DF)

This paper describes the development and validation of simple and selective analytical method for determination of 3.4-methylenedioxymethamphetamine (MDMA) in Ecstasy tablets, using high performance liquid chromatography with fluorescence detection. Analysis was performed in a reversed phase column (LiChrospher 100 C18, 150 x 4.6 mm, 5 µm), isocratic elution with phosphate buffer 25 mmol/L pH 3.0 and acetonitrile (95:5, v/v). The method presents adequate linearity, selectivity, precision and accuracy. MDMA concentration in analyzed tablets showed a remarkable variability (from 8.5 to 59.5 mg/tablet) although the tablet weights were uniform, indicating poor manufacturing control thus imposing additional health risks to the users.

Determinação de ácido valpróico em soro por cromatografia líquida de alta eficiência com detector de arranjo de diodos (CLAE-DAD), após derivatização com brometo de fenacila

Valproic acid (VA) is a drug used to control seizures in several epileptic conditions. In VA pharmacotherapy, therapeutic drug monitoring is recommended to obtain adequate seizure control and avoid toxicity. The aim of this study was to validate a method for the determination of valproic acid in serum, employing high performance liquid chromatography with diode array detection (HPLC-DAD), after derivatization with phenacyl bromide. The calibration curve (y=0.0133x-0.0025) presented good linearity with r²=0.9999. Accuracy (101-115%), intra-assay precision (4.53-8.15%) and inter-assay precision (3.15-6.77%) were acceptable. The quantification limit was 2.0 µg/mL. The method presented similar results to enzyme immunoassay.

Un método reproducible para obtener peg biramificado monofuncional de alta pureza

PEGylation has become a widely applied technique to enhancing in vitro and in vivo stability of therapeutic proteins and to increasing materials biocompatibility. PEG branched structures have proven useful for protein and peptide modification. Furthermore, they may be better than linear structures for many purposes. This paper describes an improved procedure for obtaining 2-arms PEG based on L-lysine. The efficiency of the synthesis was not related to moisture of the raw materials. This procedure does not use hazardous reagents as previous protocols do. It implemented a purification process for obtaining the desired structure with high purity ( > 99%). Finally, the procedure described here allows the obtaining of others PEGylation reagents.