Unitermos: Isofl avonas, genisteína, daidzeína, gliciteína, CCD, CLAE.ABSTRACT: "Determination of daidzein, genistein and glycitein in isofl avone capsules by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC)". The use of herbal products and supplements based on isofl avone dry extracts has increased considerably in the last decade, mainly due to benefi cial effects to relief of the menopausal symptoms credited to those compounds. Genistein, daidzein and glycitein are the most abundant isofl avone aglycones found in soy extract, where they also occur as glycosides. Concerning their uses, there is neither standardization regarding the minimum content of each aglycone in the extracts or capsules, nor an offi cial method to the quality control of these products. The present work presents a TLC method for qualitative analysis of the three aglycones and their glycosides in extracts and capsules of isofl avones, before and after acid hydrolysis. The quantitative analysis of the isofl avone capsules, carried out by high performance liquid chromatography (HPLC), showed high variation in the content of the three aglycones, after acid hydrolysis. The contents varied in the following way, in the 18 batches of evaluated capsules: daidzein (13.34 to 76.20 mg/ capsule), genistein (0.61 to 27.18 mg/capsule) and glycitein (0.49 to 8.80 mg/capsule).Keywords: Isofl avones, genistein, daidzein, glycitein, TLC, HPLC. INTRODUÇÃONos últimos anos, os fi toestrógenos têm sido alvo de vários estudos, devido à sua possível atividade estrogênica (Anderson et al., 1999). As isofl avonas são os fi toestrógenos mais comuns, sendo encontradas em abundância nos grãos de soja (Glycine max L.) e seus derivados. Daidzeína, genisteína e gliciteína são as isofl avonas presentes em maior proporção na soja, ocorrendo também na forma de glicosídeos, denominados daidzina, genistina e glicitina, respectivamente (Figura 1) (Duncan et al., 2003). Há um crescente interesse no benefício potencial das isofl avonas em vários aspectos da saúde humana, particularmente nas doenças ocidentais e crônicas, como vários tipos de cânceres hormônio-dependentes, doenças cardiovasculares, osteoporose e, principalmente, no alívio dos sintomas relacionados à menopausa (Duncan et al., 2003).Devido aos efeitos colaterais decorrentes da terapia de reposição hormonal convencional, e à alta incidência dos sintomas indesejáveis associados à menopausa, a manipulação de cápsulas contendo 617 Determinação de daidzeína, genisteína e gliciteína em cápsulas de isofl avonas por cromatografi a em camada delgada (CCD) Rev

A simple HPLC method for determination of mefloquine hydrochloride in tablets was developed and validated. The separation was carried out on an Xterra RP18 (250 × 4.6 mm id, 5 µm particle size) analytical column. The mobile phase was 0.05 M monobasic potassium phosphate buffer (pH 3.5)–methanol (40 + 60, v/v). The flow rate and wavelength were set to 1 mL/min and 283 nm, respectively. The method was specifc for mefloquine hydrochloride in the presence of hydrolytic, oxidative, and photolytic degradation products. It was also linear, precise, accurate, and robust, being suitable for routine QC analyses and stability studies. The developed HPLC method was compared to a previously described spectrophotometric method.

Background Cryptococcosis affects more than 220,000 patients/year, with high mortality even when the standard treatment [amphotericin B (AMB), 5-flucytosin (5-FC) and fluconazole] is used. AMB presents high toxicity and 5-FC is not currently available in Brazil. In a pre-clinical study, pioglitazone (PIO - an antidiabetic drug) decreased AMB toxicity and lead to an increased mice survival, reduced morbidity and fungal burden in brain and lungs. The aim of this trial is to evaluate the efficacy and safety of PIO combined with standard antifungal treatment for human cryptococcosis. Methods A phase 1/2, randomized, double blind, placebo-controlled trial will be performed with patients from Belo Horizonte, Brazil. They will be divided into three groups (placebo, PIO 15 mg/day or PIO 45 mg/day) and will receive an additional pill during the induction phase of cryptococcosis’ treatment. Our hypothesis is that treated patients will have increased survival, so the primary outcome will be the mortality rate. Patients will be monitored for survival, side effects, fungal burden and inflammatory mediators in blood and cerebrospinal fluid. The follow up will occur for up 60 days. Conclusions We expect that PIO will be an adequate adjuvant to the standard cryptococcosis’ treatment. Trial registration ICTRP/WHO (and International Clinical Trial Registry Plataform (ICTRP/WHO) ( http://apps.who.int/trialsearch/Trial2.aspx?TrialID=RBR-9fv3f4 ), RBR-9fv3f4 ( http://www.ensaiosclinicos.gov.br/rg/RBR-9fv3f4 ). UTN Number: U1111-1226-1535. Ethical approvement number: CAAE 17377019.0.0000.5149.

The development and validation of an HPLC-UV method and a microbiological assay were performed for the analysis of ketoconazole in capsule formulations. The bioassay was developed using a specific agar diffusion technique with the strain of Candida albicans ATCC 18804 as the test organism. The effect of the mobile phase pH in the range of 2.57.5 on the retention and tailing factors of the ketoconazole peak was analyzed in the chromatography method and a pH value of 4.5 was considered to be adequate. A prospective validation of both methods showed adequate linearity (r2 > 0.99 for the two methods), precision, (RSD = 2.42 for intraday and 2.69 for interday precision for bioassay; RSD = 0.74 for intraday and 0.66 for interday precision for HPLC-UV), and accuracy (mean recoveries were 103 1.0 for bioassay and 99 1.0 for HPLC-UV). Student's t-test revealed no significant difference between the results obtained by the two methods (P < 0.05). The contents found for three capsule samples showed a strong correlation, as attested by Pearson's coefficient value (r = 0.9998), which also evidenced the concordance between the studied methodologies.

Introdução: A trazodona é um antidepressivo atípico derivado da triazolopiridina, indicado para o tratamento da depressão com ou sem episódios de ansiedade, dor associada à neuropatia diabética e outros tipos de dor crônica. Objetivo: Este estudo teve como objetivo avaliar a bioequivalência entre a formulação teste de Trazodona 100 mg (Sanofi Medley Farmacêutica Ltda) e o produto de referência, Donaren (Apsen Farmacêutica S/A) de acordo com a legislação vigente. Método: Foi realizado um estudo cruzado, aberto, randomizado, de dose única com indivíduos saudáveis ​​de ambos os sexos. A fase clínica foi realizada com 48 indivíduos que receberam os medicamentos em condições de alimentação. A fármaco foi quantificado no plasma por cromatografia líquida acoplada a espectrometria de massas (LC-MS/MS). A avaliação da bioequivalência foi baseada em critérios de aceitação pré-definidos de 80,00 – 125,00% para o intervalo de confiança de 90% para a razão dos produtos teste e referência para os dados log-transformados da área sob a curva (ASC) e da concentração plasmática máxima (Cmax), conforme recomendação da Anvisa. Resultados: As razões geométricas médias (intervalos de confiança de 90%) para Cmax e ASC0-t foram 103,22% (96,13 – 110,84) e 99,06% (94,80 – 103,150), respectivamente. Não houve eventos adversos durante o estudo. Conclusão: As formulações teste e de referência foram consideradas estatisticamente bioequivalentes de acordo com os requisitos regulatórios. A formulação do teste tem sido disponibilizada no mercado local, contribuindo para o acesso da população a medicamentos genéricos de qualidade para o tratamento de transtornos depressivos.