Analysis of polycyclic aromatic hydrocarbons in fish: optimisation and validation of microwave-assisted extraction

An accurate and sensitive method for determination of 18 polycyclic aromatic hydrocarbons (PAHs) (16 PAHs considered by USEPA as priority pollutants, dibenzo[a,l]pyrene and benzo[j]fluoranthene) in fish samples was validated. Analysis was performed by microwave-assisted extraction and liquid chromatography with photodiode array and fluorescence detection. Response surface methodology was used to find the optimal extraction parameters. Validation of the overall methodology was performed by spiking assays at four levels and using SRM 2977. Quantification limits ranging from 0.15–27.16 ng/g wet weight were obtained. The established method was applied in edible tissues of three commonly consumed and commercially valuable fish species (sardine, chub mackerel and horse mackerel) originated from Atlantic Ocean. Variable levels of naphthalene (1.03–2.95 ng/g wet weight), fluorene (0.34–1.09 ng/g wet weight) and phenanthrene (0.34–3.54 ng/g wet weight) were detected in the analysed samples. None of the samples contained detectable amounts of benzo[a]pyrene, the marker used for evaluating the occurrence and carcinogenic effects of PAHs in food.

Criteria for the validation of specialized verb equivalents : application in bilingual terminography

Multilingual terminological resources do not always include valid equivalents of legal terms for two main reasons. Firstly, legal systems can differ from one language community to another and even from one country to another because each has its own history and traditions. As a result, the non-isomorphism between legal and linguistic systems may render the identification of equivalents a particularly challenging task. Secondly, by focusing primarily on the definition of equivalence, a notion widely discussed in translation but not in terminology, the literature does not offer solid and systematic methodologies for assigning terminological equivalents. As a result, there is a lack of criteria to guide both terminologists and translators in the search and validation of equivalent terms. This problem is even more evident in the case of predicative units, such as verbs. Although some terminologists (L‘Homme 1998; Lerat 2002; Lorente 2007) have worked on specialized verbs, terminological equivalence between units that belong to this part of speech would benefit from a thorough study. By proposing a novel methodology to assign the equivalents of specialized verbs, this research aims at defining validation criteria for this kind of predicative units, so as to contribute to a better understanding of the phenomenon of terminological equivalence as well as to the development of multilingual terminography in general, and to the development of legal terminography, in particular. The study uses a Portuguese-English comparable corpus that consists of a single genre of texts, i.e. Supreme Court judgments, from which 100 Portuguese and 100 English specialized verbs were selected. The description of the verbs is based on the theory of Frame Semantics (Fillmore 1976, 1977, 1982, 1985; Fillmore and Atkins 1992), on the FrameNet methodology (Ruppenhofer et al. 2010), as well as on the methodology for compiling specialized lexical resources, such as DiCoInfo (L‘Homme 2008), developed in the Observatoire de linguistique Sens-Texte at the Université de Montréal. The research reviews contributions that have adopted the same theoretical and methodological framework to the compilation of lexical resources and proposes adaptations to the specific objectives of the project. In contrast to the top-down approach adopted by FrameNet lexicographers, the approach described here is bottom-up, i.e. verbs are first analyzed and then grouped into frames for each language separately. Specialized verbs are said to evoke a semantic frame, a sort of conceptual scenario in which a number of mandatory elements (core Frame Elements) play specific roles (e.g. ARGUER, JUDGE, LAW), but specialized verbs are often accompanied by other optional information (non-core Frame Elements), such as the criteria and reasons used by the judge to reach a decision (statutes, codes, previous decisions). The information concerning the semantic frame that each verb evokes was encoded in an xml editor and about twenty contexts illustrating the specific way each specialized verb evokes a given frame were semantically and syntactically annotated. The labels attributed to each semantic frame (e.g. [Compliance], [Verdict]) were used to group together certain synonyms, antonyms as well as equivalent terms. The research identified 165 pairs of candidate equivalents among the 200 Portuguese and English terms that were grouped together into 76 frames. 71% of the pairs of equivalents were considered full equivalents because not only do the verbs evoke the same conceptual scenario but their actantial structures, the linguistic realizations of the actants and their syntactic patterns were similar. 29% of the pairs of equivalents did not entirely meet these criteria and were considered partial equivalents. Reasons for partial equivalence are provided along with illustrative examples. Finally, the study describes the semasiological and onomasiological entry points that JuriDiCo, the bilingual lexical resource compiled during the project, offers to future users.

Identification of oligomers in polyethyleneterephthalate bottles for mineral water and fruit juice - Development and validation of a high-performance liquid chromatographic method for the determination of first series cyclic trimer

Cyclic oligomers were identified in PET bottles used for mineral water and fruit juice using MS and H-1 and C-13 NMR: a first series cyclic trimer, a first series cyclic tetramer, a first series cyclic dimmer and a second series cyclic trimer. An analytical method to determine first series cyclic trimer in these bottles was developed and validated, using HPLC. The first series cyclic trimer levels were 316-462 mg/100 g of PET bottle. (c) 2005 Elsevier B.V. All rights reserved.

Development and validation of a stability-indicative agar diffusion assay to determine the potency of linezolid in tablets in the presence of photodegradation products

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and Validation of a UV-Spectrophotometric Method for Determination of Flucloxacillin Sodium in Capsules

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development and validation of a new and rapid HPLC for determination of lyophilized teicoplanin

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comparative study of analytical methods by direct and first-derivative UV spectrophotometry for evaluation of losartan potassium in capsules

O losartano potássico é um agente anti-hipertensivo não peptídico, que exerce sua ação por bloqueio específico dos receptores da angiotensina II. Este trabalho propôs a validação e aplicação de métodos analíticos orientados ao controle de qualidade de losartano potássico 50 mg na forma farmacêutica cápsula, utilizando a espectrofotometria direta e derivada de primeira ordem na região do UV. Baseado nas características espectrofotométricas de losartano potássico, um sinal a 205 nm do espectro de ordem zero e um sinal a 234 nm do espectro de primeira derivada foram adequados para a quantificação. Os resultados foram usados para comparar essas duas técnicas instrumentais. O coeficiente de correlação entre as respostas e as concentrações de losartano potássico na faixa de 3,0-7,0 mg L-1 e 6,0-14,0 mg L-1 para espectrofotometria direta e derivada de primeira ordem em solução aquosa, respectivamente, foi de (r) of 0,9999 para ambos os casos. Os métodos foram aplicados para quantificação de losartano potássico em cápsulas obtidas de farmácias de manipulação locais e demonstraram ser eficientes, fáceis de aplicar e de baixo custo. Além disso, não necessitam de reagentes poluentes e requerem equipamentos economicamente viáveis.

Development, optimization and validation of gas chromatographic fingerprinting of Brazilian commercial gasoline for quality control

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Electromyographic validation of the trapezius and serratus anterior muscles in rowing exercises with middle grip

Because the lack of textbooks based on electromyographic studies in the area of exercises for physical conditioning, the authors proposed to study the trapezius (upper portion) (TS) and the serratus anterior (lower portion) (SI) muscles during the execution of four different modalities of rowing exercises with middle grip in 24 male volunteers, 18 to 25 years old. For the recordings, it was used a two-channel TECA TE 4 electromyograph and Hewlett Packard surface electrodes. For the movements, a supine bench and a 120 cm-long bar made of low weight wood were used. The results showed that TS acted significantly in upright, sitting and inclined rowing, justifying its inclusion in physical conditioning programmes, while SI, in spite of acting preferentially in upright and sitting rowing, presented activity levels which do not justify its inclusion.

Development and validation of HPLC method for quantitative analysis of triamcinolone in biodegradable microparticles

A simple, rapid, selective and specific high performance liquid chromatographic (HPLC) method for quantitative analysis of the triamcinolone in polylactide-co-glycolide acid (PLGA) microparticles was developed. The chromatographic parameters were reversed-phase C18 column, 250mm x 4.6mm, with particle size 5 μm. The column oven was thermostated at 35°C ± 2°C. The mobile phase was methanol/water 45:55 (v/v) and elution was isocratic at a flow-rate of 1 mL.mL-1. The determinations were performed using a UV-Vis detector at 239 nm. The injected sample volume was 10 μL. The standard curve was linear (r2 > 0.999) in the concentration range 100-2500 ng.mL-1. The method showed adequate precision, with a relative standard deviation (RSD) was smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The method showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantitation of triamcinolone in PLGA microparticles.

Development and validation of a microbiological agar assay for determination of orbifloxacin in pharmaceutical preparations

Orbifloxacin is a fluoroquinolone with broad-spectrum antimicrobial activity, and belongs to the third generation of quinolones. Regarding the quality control of medicines, a validated microbiological assay for determination of orbifloxacin in pharmaceutical formulations has not as yet been reported. For this purpose, this paper reports the development and validation of a simple, sensitive, accurate and reproducible agar diffusion method to quantify orbifloxacin in tablet formulations. The assay is based on the inhibitory effect of orbifloxacin upon the strain of Staphylococcus aureus ATCC 25923 used as test microorganism. The results were treated statistically by analysis of variance and were found to be linear (r = 0.9992) in the selected range of 16.0-64.0 μg/mL, precise with relative standard deviation (RSD) of repeatability intraday = 2.88%, intermediate precision RSD = 3.33%, and accurate (100.31%). The results demonstrated the validity of the proposed bioassay, which allows reliable orbifloxacin quantitation in pharmaceutical samples and therefore can be used as a useful alternative methodology for the routine quality control of this medicine. © 2011 by the authors; licensee MDPI, Basel, Switzerland.

Validation of microbiological assay for determination of cefuroxime in injectable preparations

The validation of a microbiological assay, applying agar diffusion method for determination of the active of cefuroxime in power for injection, is described. Using a strain of Micrococcus luteus ATCC 9341 as the test organism, cefuroxime was measured in concentrations ranging from 30.0 to 120.0 μg/mL. The method validation showed that it is linear (r = 0.9999), precise (relative standard deviation = 0.37%) and accurate (it measured the added quantities). Microbiological assay is satisfactory for quantitation of cefuroxime in powder for injection and the validity of the proposed bioassay, which is a simple and a useful alternative methodology for cefuroxime determination in routine quality control.

Development and validation of a successful microbiological agar assay for determination of ceftriaxone sodium in powder for injectable solution

Ceftriaxone sodium is a cephalosporin with broad-spectrum antimicrobial activity and belongs to the third generation of cephalosporins. Regarding the quality control of medicines, a validated microbiological assay for the determination of ceftriaxone sodium in powder for injectable solution has not been reported yet. This paper reports the development and validation of a simple, accurate and reproducible agar diffusion method to quantify ceftriaxone sodium in powder for injectable solution. The assay is based on the inhibitory effect of ceftriaxone sodium on the strain of Bacillus subtilis ATCC 9371 IAL 1027 used as test microorganism. The results were treated statistically by analysis of variance and were found to be linear (r = 0.999) in the selected range of 15.0-60.0 μg/mL, precise with a relative standard deviation (RSD) of repeatability intraday = 1.40%, accurate (100.46%) and robust with a RSD lower than 1.28%. The results demonstrated the validity of the proposed bioassay, which allows reliable ceftriaxone sodium quantitation in pharmaceutical samples and therefore can be used as a useful alternative methodology for the routine quality control of this medicine. © 2012 by the authors; licensee MDPI, Basel, Switzerland.