Determination of ochratoxin A in coriander (Coriandrum sativum L.) by HPCL/fluorescence detection

An analytical study based on extraction with acetonitrile-water, immunoaffinity column cleanup, and HPLC/fluorescence detection for separation and identification of ochratoxin A in coriander was carried out. Validation of the applied methodology was done through accuracy and precision studies. Homogenized samples of coriander were spiked in triplicate with ochratoxin A at 0.5, 1.0, 2.0, and 5.0 µg/kg levels. Recovery values were in the range of 98% for a fortification level at 0.5 µg/kg to 109.1% at 1.0 µg/kg. Application to coriander samples available in Portuguese markes showed no contamination with ochratoxin A.

Tarkkuuselektroniikkatuotteen elinkaariarviointi tuotesuunnittelun tueksi

Tämän diplomityön tarkoituksena oli tutkia tarkkuuselektroniikkatuotteen ympäristönäkökohtia elinkaariarvioinnin avulla. Työn osana tehtiin elinkaariarviointi (LCA) kahdelle tarkkuuselektroniikkatuotteelle. LCA:ssa keskityttiin elinkaaren kehdosta-asiakkaalle-vaiheisiin. Työn tavoitteena oli tuottaa määrällistä ja laadullista tietoa valittujen tuotteiden ympäristövaikutuksista. Selvitys tehtiin yrityksen tuotesuunnittelun tueksi. LCA:n inventaarioanalyysiin kerättiin prosessikohtaista tietoa selvityksen aikana. Myös kaupallista LCA-ohjelmaa ja sen tarjoamia tietopankkeja hyödynnettiin elinkaariarvioinnin toteuttamisessa. Teoriaosassa esitellään LCA-menetelmä. Lisäksi tarkastellaan elinkaariarviointiin liittyviä tuotekohtaisia ympäristökysymyksiä. Työssä eritellään myös yleisesti tarkkuuselektroniikkatuotteen eri osien elinkaareen vaiheita ja niihin liittyviä ympäristönäkökohtia. Kokeellisessa osassa kuvataan kahdelle tuotteelle tehtyä LCA-tapaustutkimusta. Elinkaariarvioinnin inventaariotiedon lähteet kuvataan. Inventaarioanalyysin ja vaikutusarvioinnin avulla tuodaan esille tuotteiden ympäristökuormaan merkittävimmin vaikuttavat prosessit ja elinkaaren vaiheet. Lisäksi tarkastellaan miten tapaustuotteiden ympäristökuormaa voitaisiin pienentää kahden esimerkin avulla. Lopuksi annetaan suosituksia jatkotoimenpiteistä tuotesuunnitteluun ja tiedonkeruuseen.

Determinação de lamivudina, estavudina e nevirapina, em comprimidos, por cromatografia líquida de alta eficiência

A high performance liquid chromatography method was developed to quantify lamivudine, stavudine and nevirapine combined in tablets. The separation was carried out in less than 10 min using a phosphate buffer of pH 3.0 and acetonitrile (75:25, v/v) as mobile phase, a LiChrospher ODS column and UV detection at 266 nm. The method was linear over the range of 15-135 µg/mL (lamivudine), 4-36 µg/mL (stavudine) and 20-180 µg/mL (nevirapine). The accuracy ranged from 98.56 to 102.04% and intra-day and inter-day precision was less than 1% for the three drugs. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.

Determinação de contaminantes em óleos lubrificantes usados e em esgotos contaminados por esses lubrificantes

A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of Zn, Fe, Pb, Ni and Cu by the flame atomic absorption spectrometry technique. Sulphanilic acid was added to oil samples, the mixture coked and the coke ashed at 550 ºC. The solutions of the ash were analysed by flame AAS for these metals. The quantification limits were 38.250 µg g-1 for Zn, 4.550 µg g-1 for Fe, 1.562 µg g-1 for Pb, 1.450 µg g-1 for Ni, and 0.439 µg g-1 for Cu. The determinations, in lubricating oil, showed good precision and accuracy with recoveries between 90 and 110 %, indicating a negligible matrix effect in the experiments using addition of analyte, with relative standard deviation lower than 5%. The results for analysis of wastewater contamined by theses lubricants showed a very high relative standard deviation.

Desenvolvimento e validação de um método analítico para a determinação de histamina em vinhos utilizando cromatografia líquida de alta eficiência com detecção por fluorescência

A rapid and efficient method for the analysis of histamine in wines using HPLC with fluorescence detection after derivatization was developed and validated. The method LOD and LOQ values were 0.25 and 0.50 mg L-1 respectively. The repeatability and intermediary precision for the instrument and for the method presented RSD values of 3.7 and 2.9%, and 6.0 and 5.6%, respectively. The recoveries were 95.5 and 89.9% for the fortification levels of 2 and 10 mg L-1. The method was applied to determine the histamine content in Cabernet Sauvignon wines, which presented values between 1.2 and 5.7 mg L-1.

Ensaio de proficiência para análise de ditiocarbamatos em polpa de banana

A proficiency assay of the determination of dithiocarbamate pesticide residues in banana was carried out. Fourteen laboratories participated in this study. Homogeneity and stability testing were performed by INCQS on the samples sent to the laboratories. Analytical results supplied by the pesticide residues laboratory of the VWA/KvW, Amsterdam, Holland, were used to define the designated value for the thiram concentration in the study samples. RESULTS: Fifty percent of the participating laboratories had satisfactory results. Efforts are needed to improve the precision of the analytical results and to decrease the number of false negative results observed.

Determinação espectrofotométrica simultânea de paracetamol e ibuprofeno em formulações farmacêuticas usando calibração multivariada

A simple method was proposed for determination of paracetamol and ibuprofen in tablets, based on UV measurements and partial least squares. The procedure was performed at pH 10.5, in the concentration ranges 3.00-15.00 µg ml-1 (paracetamol) and 2.40-12.00 µg ml-1 (ibuprofen). The model was able to predict paracetamol and ibuprofen in synthetic mixtures with root mean squares errors of prediction of 0.12 and 0.17 µg ml-1, respectively. Figures of merit (sensitivity, limit of detection and precision) were also estimated. The results achieved for the determination of these drugs in pharmaceutical formulations were in agreement with label claims and verified by HPLC.

Otimização e validação da técnica de extração líquido-líquido com partição em baixa temperatura (ELL-PBT) para piretróides em água e análise por CG

The liquid-liquid extraction with the low temperature partition technique was developed for the analysis of four pyrethroids in water by CG. Using a factorial design the extraction technique was optimised evaluating the effect of the variables ionic strength, contact time and proportion between sample and solvent volumes. The validation parameters sensitivity, precision, accuracy and detection and quantification limits were evaluated. The LOD and LOQ of the method varied from 1.1 to 3.2 µg L-1 and 2.7 to 9.5 µg L-1, respectively.

Influência de desproteinizantes ácidos na quantificação da glutationa reduzida eritrocitária por CLAE-UV

Large differences in reduced glutathione (GSH) levels have been found in different investigations, also in healthy people. GSH oxidation in vitro has been associated with sample acidification in the presence of oxihemoglobin. In this work, the influence of different acids on GSH determination utilizing HPLC with UV detection was evaluated. The results showed that metaphosphoric acid and sulfosalicylic acid were inadequate for analysis, because metaphosphoric acid showed to be inefficient for deproteinization and with sulfosalicylic acid loss of GSH was observed. Trichloroacetic acid did not effect GSH quantification, since the deproteinized form was immediately derivatized with 5, 5´-dithio-bis (2-nitrobenzoic) acid. Methods with TCA deproteinization presented linear results from 0.5 to 3.0 mM. The correlation coefficient between aqueous curves and GSH spiked RBC exceeded 0.99. Precision calculations showed CV lower than 10% and bias within ± 10% for concentrations of 0.5; 1.5 and 3.0 mM GSH. The recovery was higher than 94%. Moreover, GSH blood concentrations were independent of hemoglobin concentrations.

Avaliação das variáveis analíticas do método de Folin-Ciocalteu para determinação do teor de taninos totais utilizando como modelo o extrato aquoso de folhas de psidium guajava L.

The main analytical variables of a modified Folin-Ciocalteu method were studied by UV-Vis and gradient HPLC-PDA methods, using purified (PC) and technical grade (TGC) casein. Rutin and an aqueous extract of Psidium guajava L. leaves were used as models. The best results were ascribed to TGC. Certainly PC bonds the polyphenols of the P. guajava extract better than TGC, but TGC afforded better precision. A lack of specificity occurred when rutin was analyzed together with the P guajava extract. Additional analyses performed with the flavonoid fraction of P. guajava extract by HPLC-PDA had confirmed that casein was able to bind catechin, gallic acid and P. guajava flavonoids in a non-specific way.

Determinação do teor de edta remanescente em soluções de limpeza de equipamentos industriais

Cleaning solutions containing EDTA are widely employed to remove incrustation despite of the costs involved. The free content of EDTA in commercial solutions may be determined by mixing an aliquot to ammonium oxalate and using a standard calcium solution as titrant. The end-point is detected by the formation of insoluble calcium oxalate after all EDTA is complexed. A system for turbidimetric detection of the end-point was envisaged to substitute the visual detection, which impaired the analyses of dark samples. The proposed method was tested with real samples and good accuracy and precision was obtained.

Dissolution test for glibenclamide tablets

The aim of this work is to develop and validate a dissolution test for glibenclamide tablets. Optimal conditions to carry out the dissolution test are 500 mL of phosphate buffer at pH 8.0, paddles at 75 rpm stirring speed, time test set to 60 min and using equipment with six vessels. The derivative UV spectrophotometric method for determination of glibenclamide released was developed, validated and compared with the HPLC method. The UVDS method presents linearity (r² = 0.9999) in the concentration range of 5-14 µg/mL. Precision and recoveries were 0.42% and 100.25%, respectively. The method was applied to three products commercially available on the Brazilian market.

Validação de método por cromatografia líquida de alta eficiência para determinação da lamivudina e zidovudina em comprimidos

An HPLC method was validated to assay lamivudine and zidovudine combined in tablets. The chromatographic separation was carried out using methanol and acetate buffer pH 6.5 (50:50 v/v) and a RP-18 column, as mobile and stationary phase, respectively. The UV detection was at 270 nm. The method was linear in the range of 24 - 36 µg/mL (lamivudine) and 48 - 72 µg/mL (zidovudine). The recovery (accuracy) ranged from 101.35% to 103.04% and the precision (repeatability and intermediate precision) was less than 2%. The method can be also applied to the quantification of these drugs in the dissolution test of tablets containing both drugs.

Reversed phase HPLC determination of tamoxifen in dog plasma and its pharmaco-kinetics after a single oral dose administration

The analytical method developed to evaluate tamoxifen in dog plasma samples was precise, accurate, robust and linear in the range of 5-200 ng/mL. The limits of detection and quantification were 0.981 ng/mL and 2.97 ng/mL, respectively. Besides, the intra-day precision and accuracy variations were 8.78 and 10.16%, respectively. Tamoxifen concentrations were analyzed by combined reversed phase liquid chromatography and UV detection (lambda=280 nm). The study was conducted using an open randomized 2-period crossover balanced design with a 1-week washout period between the doses. This simple, rapid and selective method is suitable for pharmacokinetic, bioavailability and bioequivalence studies.

Heavy atom enhanced room-temperature phosphorimetry for ultratrace determination of harmane

Harmane has been proposed for the treatment of epilepsy, AIDS and leshmaniosis. Its room-temperature phosphorescence was induced using either AgNO3 or TlNO3, enabling absolute limits of detection of 0.12 and 2.4 ng respectively, with linear dynamic ranges extending up to 456 ng (AgNO3) and 911 ng (TlNO3). Relative standard deviations around 3% were observed for substrates containing 46 ng of harmane. Such sensitivity and precision are needed because harmane intake must be strictly controlled to achieve proper therapeutic response. Interference studies were performed using thalidomide, reserpine and yohimbine. Recovery of 104±6% was achieved using solid surface room-temperature phosphorimetry. The result was comparable to the one obtained by micellar electrokinetic chromatography.