Desenvolvimento e validação de método analítico para determinação de teor de ácido gálico e catequina no fitoterápico sanativo® por cromatografia líquida de alta eficiência

The herbal medicine Sanativo® is produced by the Pernambucano Laboratory since 1888 with indications of healing and hemostasis. It is composed of a fluid extract about Piptadenia colubrina, Schinus terebinthifolius, Cereus peruvianus and Physalis angulata. Among the plants in their composition, S. terebinthifolius and P. colubrina have in common phenolic compounds which are assigned most of its pharmacological effects. The tannins, gallic acid and catechin were selected as markers for quality control. The aim of this study was the development and validation of analytical method by HPLC/UV/DAD for the separation and simultaneous quantification of gallic acid (GAC) and catechin (CTQ) in Sanativo®. The chromatographic system was to stationary phase, C-18 RP column, 4,6 x 150 mm (5 mm) under a temperature of 35 ° C, detection at 270 and 210 nm. The mobile phase consisted of 0.05% trifluoroacetic acid and methanol in the proportions 88:12 (v/v), a flow rate of 1 ml/min. The analytical method presented a retention factor of 0.30 and 1.36, tail factor of 1.8 and 1.63 for gallic acid and catechin, respectively, resolution of 18.2, and theoretical plates above 2000. The method validation parameters met the requirements of Resolution n º 899 of May 29, 2003, ANVISA. The correlation coefficient of linear regression analysis for GAC and CTQ from the standard solution was 0.9958 and 0.9973 and when performed from the Sanativo® 0.9973 and 0.9936, the matrix does not interfere in the range 70 to 110 %. The limits of detection and quantification for GAC and CQT were 3.25 and 0.863, and 9.57 and 2.55 mg/mL, respectively. The markers, GAC and CQT, showed repetibility (coefficient of variation of 0.94 % and 2.36 %) and satisfactory recovery (100.02 ± 1.11 % and 101.32 ± 1.36 %). The method has been characterized selective and robust quantification of GAC and CTQ in the Sanativo® and was considered validated

Caracterização e quantificação de marcadores químicos do extrato hidroetanólico das folhas de Kalanchoe brasiliensis Cambess

Kalanchoe brasiliensis Cambess (Crassulaceae), commonly known as saião , coirama branca , folha grossa , is originally from Brazil and commonly found in São Paulo to Bahia, mainly in the coastal zone. Regarding of biological activities, most preclinical studies were found in the literature, mainly about the anti-inflammatory activity of extracts obtained from leaves and / or aerial parts of K. brasiliensis. As regards the chemical constitution, it has been reported mainly the presence of flavonoids in the leaves of the species, but until this moment did not knows which are the active compounds. Although it is a species widely used in traditional medicine in Brazil, there is no monograph about the quality parameters of the plant drug. In this context, this study aims to characterize and quantify the chemical markers of hydroethanolic extract (HE) from the leaves of K. brasiliensis, which can be used in quality control of plant drug and derivatives obtained from this species. The methodology was divided into two parts: i. Phytochemical study: to fractionate, isolate and characterizate of the chemical (s) marker (s) of the HE from the leaves of K. brasiliensis; ii. To Developed validate of analytical method by High Performance Liquid Chromatography (HPLC)-diode array detector (DAD) to quantify the chemical (s) marker (s) of the EH. i. The EH 50% was prepared by turbo extraction method. It was then submitted to liquid-liquid partition, obtaining dichloromethane, n-butanol and ethyl acetate (AcOEt) fractions. The AcOEt fraction was selected to continue the fractionation process, because it has a chemical profile rich in flavonoids. The acOEt fraction was submitted to column chromatography using different systems for obtaining the compound Kb1. To identify this compound, it was submitted to UV analysis ii. For quantitative analysis, the EH was analyzed by HPLC, using different methods. After selecting the most appropriate method, which showed satisfactory resolution and symmetrical peaks, it was validated according to parameters in the RE 899/2003. As result, it was obtained from the AcOEt fraction the compound Kb1 (2.7 mg). Until this moment, the basic nucleus was characterized by UV analysis using shift reagents. The partial chemical structure of the compound Kb1 was identified as a flavonol, containing hydroxyls in 3 , 4 position (ring A), 5 and 7 free (ring B) and a replacement of the C3 hydroxyl by a sugar. As the analysis were performed in the HPLC coupled to a DAD, we observed that the UV spectrum of the major peaks of EH from K. brasiliensis shown similar UV spectrum. According to the literature, it has been reported the presence of patuletin glycosydes derivatives in the leaves of this species. Therefore, it is suggested that the compound Kb1 is glycosylated patuletin derivative. Probably the sugar (s) unit(s) are linked in the C3 in the C ring. . Regarding the development of HPLC analytical method, the system used consists of phase A: water: formic acid (99,7:0,3, v / v) and phase B: methanol: formic acid (99,7:0,3, v / v), elution gradient of 40% B - 58% B in 50 minutes, ccolumn (Hichrom ®) C18 (250x4, 0 mm, 5 μm), flow rate 0.8 mL / min, UV detection at 370 nm, temperature 25 ° C. In the analysis performed with the co-injection of thecompound Kb1 + HE of K. brasiliensis was observed that it is one of the major compounds with a retention time of 12.47 minutes and had a content of 15.3% in EH of leaves from K. brasiliensis. The method proved to be linear, precise, accurate and reproducible. According to these results, it was observed that compound Kb1 can be used as a chemical marker of EH from leaves of K. brasiliensis, to assist in quality control of drug plant and its derivatives

Desenvolvimento e validação de método analítico para determinação de WE010, WE014 e WE017

The synthetic guanylhydrazones WE010 (3,5-di-tert-butil-4-hidroxibenzaldehyde-guanylhydrazone), WE014 (4-bifenilcarboxialdehydeguanylhydrazone) and WE017 (3,4-diclorobenzaldehydeguanylhydrazone) showed high cytotoxic activity in terms of percentage inhibition of cancer cells growth. However, further progress in the development of these drug candidates requires precise and convenient methods for their qualitative and quantitative analyses. The aim of this study was to develop and validate High Performance Liquid Chromatography with diode-array detection (HPLC-DAD) and Ultra Fast Liquid Chromatography with diode-array detection (UFLC-DAD) methods suitable for as simultaneous as isolated determination of studied guanylhydrazones, based on the optimization of chromatographic parameters and obtaining reduced detection times. The chromatographic analyses of analytes by HPLC were performed on C18 ACE analytical column (150 mm x 4.6 mm), with a particle size of 5.0 μm. Among all the conditions assayed, the best results of separation were obtained with a mixture of methanol:water (60:40, v/v) as the mobile phase at a flow rate 1.5mL/min and pH of 3.5 adjusted at acetic acid. The UFLC method was developed by experimetal desing techniques in order to find optimal chromatographic analytical conditions, which were achieved on XR-ODS analytical column (50 mm x 3.0 mm), with a particle size of 2,2 μm, maintained at 25 ºC. The mobile phase was consisted of methanol:water (65:35, v/v) with 0.1% triethylamine (TEA) and pH of 3.5 adjusted at acetic acid, at a flow rate 0.5 mL/min. The procedure were validated following evaluating parameters such as specificity, linearity, limits of detection (LD) and quantification (LQ), precision, accuracy and robustness, giving results within the acceptable range. Although the UFLC method shows better sensitivity (lower values of LD and LQ), robustness (lower rates of relative standard deviation) and minimize spending time and solvent, both developed methods were adequately applied to the analysis of guanylhydrazones molecules, may be used in routine of quality control laboratories. Keywords: guanylhydrazones, HPLC/DAD, UFLC/DAD, validation of analitical method

Qualidade microbiológica de leite UHT caprino: pesquisa de bactérias dos gêneros Staphylococcus, Bacillus e Clostridium

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Temperatura e período de exposição de sementes de milho no teste de envelhecimento acelerado

O teste de envelhecimento acelerado (EA) apresenta possibilidades de uso nos programas de controle de qualidade de sementes de milho. Porém, para uso em rotina, há necessidade de padronização das condições de temperatura e período de exposição das sementes na realização do teste. Esta pesquisa teve por objetivo avaliar o efeito da combinação de duas temperaturas (42 e 45ºC) e dois períodos de envelhecimento (72 e 96h) nos resultados do teste de envelhecimento acelerado em sementes de milho. Para isso, sementes de seis genótipos de milho, tratadas e sem tratamento fungicida, com altos valores de germinação inicial, semelhantes entre si, dentro de cada genótipo, foram submetidas ao EA, de acordo com condições de temperatura e período de exposição pré-estabelecidos. Utilizou-se o delineamento experimental inteiramente casualizado com os tratamentos (lotes x germinação, antes e após o EA) dispostos em esquema fatorial, empregando-se o teste de Tukey a 5% de probabilidade na comparação das médias. Verificou-se que sementes de milho apresentam diferenças de sensibilidade ao envelhecimento acelerado, condicionadas pelo genótipo e tratamento fungicida. Contudo, a combinação 45ºC por 72h possibilita separar lotes de qualidade fisiológica superior e inferior, independentemente do genótipo. O período de exposição das sementes ao envelhecimento acelerado determina o teor de água atingido pelas mesmas.

Envelhecimento acelerado como teste de vigor para sementes de milho e soja

A avaliação do vigor de sementes tem sido ferramenta fundamental dentro do programa de controle de qualidade, sendo o teste de envelhecimento acelerado (EA) parte importante do processo. O trabalho foi desenvolvido com o objetivo de confirmar metodologia específica para avaliação do vigor de sementes, em laboratório, tendo como base o EA. Utilizou sementes de milho e soja, seis lotes para cada espécie, com padrões de qualidade (germinação) comercialmente aceitas. As condições de envelhecimento préestabelecidas foram 42ºC/96h e 45ºC/72h para milho e 41ºC/48 e 72h e 42ºC/48 e 72h para soja. Para cada combinação de temperatura e período de envelhecimento, as sementes foram colocadas em caixas plásticas, sobre tela, com 40mL de água destilada, distribuídas em camada única e com base no peso das mesmas. O envelhecimento foi feito usando-se dois tipos de câmara, BOD e jaquetada de água (CJ). Foi determinado o teor de água (TA) e a germinação das sementes antes e após o EA. A absorção de água pelas sementes considerando-se todas as combinações de período de exposição e temperatura, as duas câmaras e as duas formas de determinação do TA, foi maior quando as sementes foram acondicionadas em camada única em relação aquelas pesadas (massa constante), usando-se a câmara jaquetada. Para o milho, a combinação de 45ºC/72h com o acondicionamento das sementes em camada única foi o método mais eficiente para a separação dos lotes quanto ao vigor. Para soja, a combinação 42ºC/48h foi mais eficiente na separação dos lotes, não havendo interferência do método de acondicionamento das sementes, na tela. Conclui-se que a camada única e a câmara tipo BOD devem ser preferencialmente utilizadas no teste EA face aos menores custos de aquisição e manutenção da BOD, visando à separação de lotes quanto aos níveis de vigor, para milho e soja.

Alternative procedure for the cold test for soybean seeds

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A utilização do controle estatístico do processo para o monitoramento do sangue: estudo de caso no Memonorte-RN

The present work is grounded basically on the use of the Basic Tools for the Statistic Process Control SPC, with the intent to detect non-conformities on a given productive process. It consists on a case study accomplished at a Hemocenter in Natal (Rio Grande do Norte). In this study it is shown that, the Statistic Process Control Technique, which was used as a tool, is useful to identify on-conformities on the volume of hemocomponents. The gathering of the used data was performed by means of document analysis, direct observations and database queries. The results achieved from the study show that the analyzed products, even though when they have presented, in some cases, points out of control, they satisfied the ANVISA standards. Finally, suggestions for further improvement of the final product and guidance for future employment of CEP, also extended to other lines of production, are presented

Importância do gerenciamento com base em dados estudo de caso : farmácias de manipulação do Estado do Rio Grande do Norte

Last century Six Sigma Strategy has been the focus of study for many scientists, between the discoveries we have the importance of data process for the free of error product manufactory. So, this work focuses on data quality importance in an enterprise. For this, a descriptive-exploratory study of seventeen pharmacies of manipulations from Rio Grande do Norte was undertaken with the objective to be able to create a base structure model to classify enterprises according to their data bases. Therefore, statistical methods such as cluster and discriminant analyses were used applied to a questionnaire built for this specific study. Data collection identified four group showing strong and weak characteristics for each group and that are differentiated from each other

Testes de vigor utilizados na avaliação da qualidade fisiológica de lotes de sementes de milho-doce (sh2)

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

Influência da dureza e potencial hidrogeniônico da calda de pulverização sobre o controle do ácaro-da-leprose em frutos de laranja doce

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A engenharia simultânea e o perfil da indústria de confecção da grande Natal/RN utilizando as ferramentas CAD/PDM e ERP

This work presents the research carried through in the industrial segment of confection of clothes of the Great Natal whose objective is to show the profile, enterprise and technological management as also the use of simultaneous engineering in the development of products. The research approaches two studies. The first one presents the current picture of the companies, synthesized through twelve variable. As, through fifteen variable it shows to the level of use of Simultaneous Engineering in the Development of Products and its amplitude in relation to the Integrated Management using tools CAD, PDM and ERP (Computer Aided Design, Product Management Date, Enterprise Resource Planning). The integration of these systems acts aiming the reduction of the cost and the development time of products. The reached results indicate that simultaneous engineering is a competitive advantage and becomes possible: to reduce the life cycle of the product, to rationalize the resources, to incorporate one high standard of the quality to the process and product as well as to personalize the product to take care of the global market. It is important to note that this work also is considered to contribute for the better understanding of the real companies situation of confection located at the Great Natal and its role in the economy of the State of the Rio Grande do Norte

Comparação da precisão dos resultados do teste de tetrazolio usando a metodologia alternativa e a tradicional em sementes de soja

The use of tetrazolium testing is recognized in the soybean seed quality control due to the large amount of data which it provides. Although it is considered a quick test, in 1998 an alternative methodology was proposed for the seed preconditioning, which allows 10 hours of time saving in seeds preparation. The objective of this research is to compare the accuracy of the new and the traditional tetrazolium testing. Three soybean seed genotypes were used, Conquista, Garantia and M-soy 8400, all 2000/2001 crop. The seeds were evaluated in relation to germination, evaluated with the traditional (TZt) and the alternative (Tza) tetrazolium test as well as with the accelerated aging performed in two different conditions (45 degrees C 24h(-1) and 45 degrees C 72h(-1)). After aging, the seeds too were submitted to TZt and Tza testing. The experimental design was a randomized blocks, with four replicates the 50 seeds per genotype in every evaluation, with exception only for tetrazolium test, with two replicates. The averages were compared in the Tukey test level of 5% probability. The comparison between the two methodologies in relation to level of vigor (class 1 to 3) and germination potential (class 1 to 5) indicated no statistical discrepancies, for aged non-aged seeds. This, the use of the alternative tetrazolium test is recommend in case a reduced seed preparation time is needed.

Controle sanitário e ambiental de um projeto de reúso em um complexo de prédios corporativos

The study that resulted in this dissertation was developed at OU RNCE PETROBRAS, in Natal, which implemented a project of rational use and reuse of water, including use of wastewater from a Sewage Treatment Plant (STP) already in place, diluted with water from own wells for irrigation of green area of the building complex corporate enterprise. Establish a methodology that can serve as guidelines for future projects controlled reuse of water like this was the objective of this research. Been proposed, implemented and evaluated three instruments of sanitary and environmental control: 1) adaptation of sewage treatment plant and quality control of the treated effluent 2) analysis of soil-nutrient interaction in the irrigated area, 3) knowledge of the local hydrogeology, especially with regard to the direction of flow of the aquifer and location of collection wells of Companhia de Águas e Esgotos do Rio Grande do Norte (CAERN) situated in the surroundings. These instruments have proven sufficient and appropriate to ensure the levels of sanitary and environmental control proposed and studied, which were: a) control of water quality off the STP and the output of the irrigation reservoir, b) control of water quality sub surface soil and assessment of progress on soil composition, c) assessment of water quality in the aquifer. For this, we must: 1) establishing the monitoring plan of the STP and its effluent quality sampling points and defining the parameters of analysis, improve the functioning of that identifying the adequacy of flow and screening as the main factors of operational control, and increase the efficiency of the station to a relatively low cost, using additional filters, 2) propose, implement and adapt simple collectors to assess the quality of water percolating into the soil of the irrigated area, 3) determine the direction of groundwater flow in the area study and select the wells for monitoring of the aquifer.

Gestão da qualidade total: introdução dos conceitos e a sua utilização em um curso para abordar o comportamento individual do aluno/profissional/cidadão

A introdução do assunto qualidade, segundo as necessidades de mercado abre espaço para a discussão da qualidade como necessidade pessoal, e também para a formação do cidadão/profissional, além de introduzir assuntos específicos de administração de empresas. Dessa forma, foi oferecida uma disciplina optativa para os alunos do Instituto de Química do Campus de Araraquara, abordando o tema Qualidade e foi denominada Gestão da Qualidade por três anos seguidos. da avaliação geral do curso extraiu-se que ele deveria ser realizado sempre, que o tema é atual e relevante e contribui para a formação profissional/pessoal. Com relação ao comprometimento com o curso de graduação, cerca de metade dos alunos assume o seu comprometimento com os estudos e os restantes dizem estarem somente envolvidos. Conclui-se, portanto que o curso atingiu os seus objetivos propostos, introduziu os principais conceitos de qualidade segundo as normas da qualidade da série ISO 9000 e suscitou a discussão da formação do aluno/profissional/cidadão.