Crescimento vegetativo de macieiras 'Fuji Suprema' sob influência da época de aplicação de proexadione cálcio

O uso de reguladores de crescimento que atuam na biossíntese de giberelinas, como o proexadione cálcio, pode possibilitar adequado balanço entre o desenvolvimento vegetativo e o reprodutivo, fundamental para a maximização dos índices produtivos. No entanto, a resposta ao uso deste regulador de crescimento depende do padrão de crescimento dos ramos. Objetivou-se com este trabalho avaliar o efeito de diferentes épocas de aplicação de proexadione cálcio no controle do desenvolvimento vegetativo de macieiras 'Fuji Suprema', sob condições climáticas do Sul do Brasil. Avaliaram-se diferentes épocas de aplicação de proexadione cálcio, a 330 g ha-1, em dois ciclos produtivos, utilizando o delineamento experimental em blocos casualizados, com dez repetições compostas por uma planta. No ciclo de 2008/2009, foram avaliadas seis épocas de aplicação (28; 58; 88; 118; 148 e 178 dias após a plena floração - DAPF). No ciclo de 2009/2010, foram avaliadas sete épocas (20; 50; 80; 110; 140; 170 e 200 DAPF), ambas comparadas com o tratamento-testemunha(sem aplicação). O proexadione cálcio em uma única aplicação, a 330 g ha-1, aplicado até 28 dias após a plena floração, pode reduzir o número, a massa e o comprimento médio dos ramos podados em macieiras 'Fuji Suprema'; porém, sobre condições que favoreçam o demasiado desenvolvimento vegetativo, o efeito mostra-se nulo. O uso de 330 g ha-1 de proexadione cálcio em uma única aplicação, indiferentemente da época de aplicação, não altera a produção de macieiras 'Fuji Suprema'.

AVALIAÇÃO FENOLÓGICA DAS DIFERENTES ESTRUTURAS DE FRUTIFICAÇÃO DAS MACIEIRAS 'GALA' E 'FUJI' NA REGIÃO DE CAÇADOR-SC

RESUMO A macieira apresenta duas fases que caracterizam seu ciclo anual: a de repouso hibernal e a de crescimento vegetativo e reprodutivo. A importância em se conhecer ainfluência das condições climáticas sobre os processos reprodutivos das plantas e em desenvolver tecnologias que minimizem os possíveis efeitos aumenta à medida que as projeções de aquecimento global se tornampreocupantes. O objetivo deste trabalho foi caracterizar o comportamento dos principais eventos fenológicos da macieira, da brotação à colheita, nas diferentes estruturas de frutificação, sob as condiçõesclimáticas do Sul do Brasil. O estudo experimental foi conduzido na Estação Experimental da Epagri (26°50’S, 50°58’W, altitude 950 m), durante os ciclos de 2011/12 e 2013/2014. As cultivares estudadas foram Gala e Fuji,com nove anos de idade, ambas sobre o porta-enxerto M9. O desenvolvimento fenológico foi observado nas diferentes estruturas de frutificação da macieira: gema de esporão, gema terminal de brindila e gemaaxilar de brindilas. As mesmas foram comparadas através dos dias e da exigência térmica necessários para a transição dos estádios, sendo contabilizados a partir do tratamento de quebra de dormência. As diferençasencontradas no início da brotação e do florescimento, entre as estruturas, dependeram consideravelmente das condições climáticas do ano em questão. Sob condições de altas temperaturas após o tratamento de quebra dedormência, houve maior sincronia fenológica entre as estruturas, sendo que sob baixas temperaturas se observou maior variabilidade dos estádios entre as mesmas. A partir do tratamento de quebra de dormência,gemas de esporões necessitam de menor acúmulo térmico para brotar, principalmente esporões de ‘Gala’ e gemas terminais de brindilas necessitam de maior acúmulo térmico que gemas de esporões para dar início aoflorescimento.

PROTETOR SOLAR DIMINUI A INCIDÊNCIA DAS PODRIDÕES ‘OLHO-D-BOI’ E ‘BRANCA’ EM MAÇÃS ‘FUJI STANDARD’ E ‘PINK LADY’

RESUMO A podridão-olho-de-boi (Cryptosporiosis perennans) e a podridão-branca (Botryosphaeria dothidea) estão entre as principais doenças de verão da macieira no Brasil. O objetivo deste trabalho foi avaliar o efeito de uma película protetora constituída de cera de carnaúba e argilas (Raynox® ), nas doses de 2,5 e 5,0%, na infecção por C. perennans e por B. dothidea em maçãs das cultivares Fuji Standard e Pink Lady. As macieiras foram pulverizadas cinco vezes de dezembro de 2007 a março de 2008, conforme previsão de condições adequadas para ocorrência dos danos e crescimento dos frutos. Na colheita, as maçãs foram inoculadas com os dois patógenos e avaliadas quanto à incidência das podridões. Indiferente à dose, o uso de Raynox® reduziu a incidência da podridão-branca e da podridão-olho-de-boi em 67% e 42% na ‘Fuji Standard’, e 43% e 42% na ‘Pink Lady’, respectivamente. O incremento da dose aumentou a eficiência do produto para o controle da podridão-olho-de-boi. Na dose de 2,5%, o controle da podridão-olho-de-boi foi de 19% e 20%, respectivamente, em maçãs ‘Fuji Standard’ e ‘Pink Lady’, enquanto para as mesmas cultivares, mas com a dose de 5,0%, estes valores foram de 65% e 63%. Mais estudos são necessários para o ajuste de dose e critérios de aplicação para que o protetor solar possa ser recomendado.

Determination of etoricoxib in human plasma using automated on-line solid-phase extraction coupled with LC-APCI/MS/MS

A liquid chromatography-tandem mass spectrometry method with atmospheric pressure chemical ionization (LC-APCI/MS/MS) was validated for the determination of etoricoxib in human plasma using antipyrin as internal standard, followed by on-line solid-phase extraction. The method was performed on a Luna C18 column and the mobile phase consisted of acetonitrile:water (95:5, v/v)/ammonium acetate (pH 4.0; 10 mM), run at a flow rate of 0.6 mL/min. The method was linear in the range of 1-5000 ng/mL (r²>0.99). The lower limit of quantitation was 1 ng/mL. The recoveries were within 93.72-96.18%. Moreover, method validation demonstrated acceptable results for the precision, accuracy and stability studies.

Development and validation of RP-LC and uv spectrophotometric methods to assay bromopride in oral and injectable solutions

A reversed-phase liquid chromatographic (LC) and ultraviolet (UV) spectrophotometric methods were developed and validated for the assay of bromopride in oral and injectable solutions. The methods were validated according to ICH guideline. Both methods were linear in the range between 5-25 μg mL-1 (y = 41837x - 5103.4, r = 0.9996 and y = 0.0284x - 0.0351, r = 1, respectively). The statistical analysis showed no significant difference between the results obtained by the two methods. The proposed methods were found to be simple, rapid, precise, accurate, and sensitive. The LC and UV methods can be used in the routine quantitative analysis of bromopride in oral and injectable solutions.

Development and validation of a LC-method for the determination of phenols in a pharmaceutical formulation containing extracts from Stryphnodendron adstringens

A sensitive RP-HPLC method with UV detection successfully measured phenol(s) in an ointment containing 3% Stryphnodendron adstringens extract. Chromatography used acetonitrile (0.05% trifluoroacetic acid):water (0.05% trifluoroacetic acid) (v/v), flow rate 0.8 mL min-1. Quantitation was accomplished by the external-standard method. Linearity for 2.00 to 16.00 μg mL-1 (gallic acid) and 1.14 to 18.24 μg mL-1 (gallocatechin) was established. Intra- and inter-day precision levels were under 5%. LOD and LOQ were 0.231 and 0.770 μg mL-1 (gallic acid) and 0.151 and 0.504 μg mL-1 (gallocatechin), respectively. Determination of phenols was unaffected by product excipients.

Evaluation of sample processing methods for the polar contaminant analysis of sewage sludge using liquid chromatography - mass spectrometry (LC/MS)

Monitoring of sewage sludge has proved the presence of many polar anthropogenic pollutants since LC/MS techniques came into routine use. While advanced techniques may improve characterizations, flawed sample processing procedures, however, may disturb or disguise the presence and fate of many target compounds present in this type of complex matrix before analytical process starts. Freeze-drying or oven-drying, in combination with centrifugation or filtration as sample processing techniques were performed followed by visual pattern recognition of target compounds for assessment of pretreatment processes. The results shown that oven-drying affected the sludge characterization, while freeze-drying led to less analytical misinterpretations.

Terbinafine: optimization of a LC method for quantitative analysis in pharmaceutical formulations and its application for a tablet dissolution test

A simple liquid chromatographic method was optimized for the quantitative determination of terbinafine in pharmaceutical hydroalcoholic solutions and tablets, and was also employed for a tablet dissolution test. The analysis was carried out using a RP-C18 (250 mm × 4.6 mm, 5 μm) Vertical® column, UV-Vis detection at 254 nm, and a methanol-water (95:5, v/v) mobile phase at a flow-rate of 1.2 mL min-1. Method validation investigated parameters such as linearity, precision, accuracy, robustness and specificity, which gave results within the acceptable range. The tablets dissolution was quite fast: 80% of the drug was dissolved within 15 min.

Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

A LC-ESI-MS/MS method was developed and validated according to the European Union decision 2002/657/EC, for the determination of tetracyclines (TCs) in chicken-muscle since Europe is one of the main markets for Brazilian products. Linearity of r > 0.9979, limits of quantification in the range of 7.0-35.0 ng/g, average recoveries of 89.38 - 106.27%, within-day and between-day precision were adequate for all TCs. The decision limit and the detection capability were 93.00-106.46 ng/g and 95.84-114.38 ng/g, respectively. This method is suitable for application in surveillance programmes of residues of TCs in chicken-muscle samples.

Otimização e validação de método empregando quechers modificado e lc-esi-ms/ms para determinação de agrotóxicos em cebola

An evaluation of the pesticides extraction from onion using a modern sample preparation method (QuEChERS) and determination by liquid chromatography tandem mass spectrometry was carried out. All the calibration curves showed r>0.99. The recoveries ranged between 61.8 and 120.0% with relative standard deviation lower than 20% for all compounds. Due to the occurrence of matrix effect, the quantification was performed using matrix-matched calibration. The limits of quantification of the method were between 0.0005 and 0.05 mg kg-1. The method shows the advantages of not require the clean-up step and consume low volume of organic solvents, decreasing time, costs and residues.

A sensitive and robust lc-ms/ms method with monolithic column and electrospray ionization for the quantitation of efavirenz in human plasma: application to a bioequivalence study

An LC-MS/MS method has been developed for the determination of efavirenz (EFZ) in human plasma using hydrochlorothiazide as internal standard (I.S.). An ESI negative mode with multiple reaction-monitoring was used monitoring the transitions m/z 313.88→69.24 (EFZ) and 296.02→204.76 (I.S.). Samples were extracted using liquid-liquid extraction. The total run time was 2.0 min. The separation was achieved with HPLC-RP using a monolithic column. The assay was linear in the concentration range of 100 - 5000 ng mL-1. The mean recovery was 83%. Intra- and inter-day precision were < 9.5% and < 8.9%, respectively and accuracy was in the range ± 8.33%. The method was successfully applied to a bioequivalence study.

Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g-1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

Set-up of a method using LC-UV to assay mometasone furoate in pharmaceutical dosage forms

A reliable method using LC-UV to assay mometasone furoate (MF) in creams or nasal sprays using the same chromatographic conditions was set up. Methanol:water 80:20 (v/v) (1.0 mL min-1) was used as mobile phase. MF was detected at 248 nm and analyzed in a concentration range from 1.0 to 20.0 µg mL-1. The method provided acceptable theoretical plates, peak simmetry, peak tailing factor and peak resolution a short run (5 min). The method showed specificity, good linearity (r = 0.9999) and the quantification limit was 0.379 µg mL-1. Furthermore, the method was precise (RSD < 2.0%), accurate (recovery > 97%) and robust.

Stability-indicating comparative methods using mekc and lc for determination of olmesartan medoxomil

A stability-indicating method using MEKC was validated for the analysis of olmesartan medoxomil in tablets. Successful separation was achieved using a fused silica capillary (40 cm x 50 µm i.d.); background electrolyte consisted of a combination of 10 mmol L-1 borate buffer and 5 mmol L-1 anionic detergent sodium dodecyl sulfate (95:5; v/v) pH 6.5; hydrodynamic mode at 50 mBar for 5 s; 25 kV separation voltage at 25 ºC; and column temperature 25 ºC with detection at 257 nm. The proposed method, validated following ICH guidelines, was applied to the determination of this antihypertensive with good results compared with an LC method.

LC/ESI-MS method applied to characterization of flavonoids glycosides in B. forficata subsp. pruinosa

Bauhinia forficata is used in folk medicine for its hypoglycemiant effect. In the south of Brazil, the subspecies pruinosa is found in a region with the characteristic flora, pampa biome. This species has been consumed by the local population as a tea for diabetes treatment. We studied the chemical composition of hydroethanolic extracts using LC/ESI-MS. The leaf extracts were prepared by percolation with 50% (v/v) ethanol. The chromatographic analyses were performed using a reverse-phase system, gradient elution with acetonitrile:phosphoric acid 0.05%, and ESI-MS in the positive ion mode. The chemical profile of the flavonoids was suggested to involve four quercetin and kaempferol glycosides.