Rapid spot test analysis for the detection of urotropine in pharmaceutical preparations

The widespread falsification and/or adulteration of commercially available pharmaceutical preparations call for reliable methods of drug identification, preferably through selective and rapid sorting color tests that could be undertaken with minimum equipment remote from laboratory facilities. The present work deals with a convenient adaptation and refinement of a spot test devised by Feigl (1966) for urotropine, based on the hydrolytic cleavage of that substance in the presence of sulfuric acid, splitting out formaldehyde which is identified by its color reaction with chromotropic acid. A simple emergency kit was developed for the quick, efficient, inexpensive and easy performance of urotropine tests by semiskilled personnel even in the drugstore laboratory (or office) as well as in a mobile screening operation. It is shown that when the reagents are added according to the recommended sequence a self-heating system is generated, increasing substantially the reactions' rates and the test sensitivity as well. The identification limit found was 25 mug of urotropine, for both solid and liquid samples. The possible interference of 84 substances/materials was investigated. Interference was noted only for methylene blue, acriflavine, Ponceau Red, Bordeaux Red (these dyes are often included in urotropine dosage forms), pyramidone, dipyrone, quinine and tetracycline. A simple procedure for removing most of the interferences is described. Data for 8 commercial dosage forms and results obtained from their analysis are presented.

Validity and reproducibility of a laser fluorescence system for detecting the activity of white-spot lesions on free smooth surfaces in vivo

The aim of the study was to determine the reproducibility and validity of DIAGNOdent in detecting active and arrested caries lesions on free smooth surfaces. Volunteers were selected from state schools of Piracicaba, São Paulo, Brazil. Overall, 220 lesions were clinically examined. Two specially trained ('calibrated') examiners performed both clinical and laser evaluations independently, and after a 1-week interval, the examinations were repeated, the intra-examiner agreement for the laser evaluation was substantial (kappa(ex1) = 0.79, kappa(ex2) = 0.71). There was almost perfect agreement between the two examiners for the clinical examination (kappa(ex1) = 0.95, kappa(ex2) = 0.85). The inter-examiner agreement showed substantial reproducibility (kappa = 0.77) for the laser examination and almost perfect agreement (kappa = 0.85) for the clinical evaluation. The validation criterion was the clinical examination of white spots, recorded as active or arrested. The sensitivity was 0.72 and the specificity was 0.73, which indicates that the DIAGNOdent was a good auxiliary method for detecting incipient caries lesions on free smooth surfaces. The utilization of both methods can improve the efficacy of caries diagnosis. Copyright (C) 2002 S. Karger AG, Basel.

Efficacy of pre- and postinoculation application of Fungicides to expanding young citrus leaves for control of melanose, scab, and alternarial brown spot

In greenhouse trials, copper hydroxide, pyraclostrobin, and famoxadone were applied to actively crowing young citrus seedlings to determine the duration of protection of young leaves provided by these fungicides against melanose, caused by Diaporthe citri, citrus scab, caused by Elsinoe fawcettii, and Alternaria brown spot, caused by Alternaria alternata. Fungicides were applied to different sets of potted plants of grapefruit for control of melanose, of rough lemon for control of scab, and of Dancy tangerine for control of Afternaria brown spot 1 to 6 days prior to inoculation. as well as on the day of inoculation. Leaf area of treated shoots was estimated on the day of fungicide application and the day of inoculation and disease severity evaluated subsequently. In most cases. copper hydroxide and famoxadone provided at least 50% control of all three diseases for only about 2 days after application. Generally, there was little or no disease control when the products were applied 4 or more days before inoculation. In contrast, pyraclostrobin usually provided a high level of control of all three diseases when applied up to 5 days prior to inoculation. The level of disease control decreased as the interval between a fungicide application and inoculation increased and the relationship between disease control and leaf expansion best fit a quadratic equation. Effective disease control was observed with copper hydroxide and famoxadone until leaf area had increased by 100 to 200%, whereas control with pyraclostrobin was observed up to 400 to 500% increase in leaf area. In postinoculation tests with scab and melanose, pyraclostrobin provided high levels of disease control (>75%) when applied up to 2 days after inoculation. whereas copper hydroxide and famoxadone had minimal postinoculation activity. Applications of pyraclostrobin to the spring flush growth of citrus trees are much more likely to provide control of melanose, scab, and Alternaria brown spot than those of famoxadone or copper hydroxide.

Effect of lesion age, humidity, and fungicide application on sporulation of Alternaria alternata, the cause of brown spot of tangerine

Alternaria brown spot, caused by Alternaria alternata, causes yield losses and fruit blemishes on many tangerines and their hybrids in most citrus areas of the world where susceptible cultivars are grown. Although the conditions affecting infection and disease severity are known, little information is available on inoculum production on infected tissue. We found that sporulation on leaves began about 10 days after symptoms developed, was abundant from 20 to 40 days, and declined thereafter. Conidial production was far greater on leaf than on fruit or twig lesions. Spore production per unit area of leaf lesion was greater on the more susceptible hybrids, Minneola and Orlando tangelos, than on the less susceptible Murcott tangor. At 74% relative humidity, conidial production on leaf lesions was low, but it was abundant at 85, 92.5, 96, and 100%. Application of Q(o)I or copper fungicides, but not ferbam, suppressed sporulation on leaf lesions for about 14 to 21 days after application. Additional applications did not appear to be more effective than a single spray in reducing inoculum production.

Determination of methyldopa in pharmaceutical formulations by combined spot test-diffuse reflectance spectroscopy

This paper describes a very simple and rapid quantitative reflectance spot test procedure for the determination of methyldopa in pharmaceutical formulations. This method is based on the complexation reaction of methyldopa with molybdate ions yielding a yellow stable complex on filter paper. Reflectance measurements were carried out at 410 nm. Under optimal conditions, the calibration graphs obtained for methyldopa by plotting the optical density of the reflectance signal (A R) vs. the log of the concentration were linear from 6.30 × 10 -3 to 1.89 × 10 -2 mol L -1, with a correlation coefficient of 0.998. The detection limit was 2.74 × 10 -3 mol L -1 (R.S.D. = 1.02%) for methyldopa. The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine metyldopa in commercial pharmaceutical formulations. The results obtained by the proposed method compare favorably with those obtained by an official procedure at 95% confidence level. ©2006 Sociedade Brasileira de Química.

Impact of climate change on the phoma leaf spot of coffee in Brazil

The potential impact of global climate change on the spatial-temporal distribution of phoma leaf spot of coffee in Brazil was evaluated. Maps were prepared with the favorability of the climate to the occurrence of the disease in the current period and future. The future scenarios used were centered for the decades of 2010-2030, 2040-2060, and 2070-2090 (scenarios A2 and B2). These scenarios were obtained from six global climate models (GCM's) provided by the Intergovernmental Panel on Climate Change (IPCC). Assuming the future scenarios outlined by the IPCC, a reduction will occur in the occurrence of climatic favorability of phoma leaf spot in Brazil in both future scenarios (A2 and B2). As with the temporal distribution, the period of greatest risk of phoma leaf spot will tend to diminish in future decades. These planned changes will be larger in the A2 scenario compared to the predicted scenario B2. Despite the decrease in the favorability of phoma leaf spot in the country, some regions still present a potential risk of this disease. Furthermore, the increased frequency of extreme weather was not taken in to account. These will certainly influence the magnitude of potential impacts of climate change on the phoma leaf spot in Brazil.

Rapid determination of furosemide by combined spot test/diffuse reflectance spectroscopy to detect doping in sport

This paper describes the development and application of a simple, cheap, and clean method for the quantification of furosemide in urine samples from athletes, to detect doping, using a combined spot test/diffuse reflectance spectroscopy procedure. The method is based on the complexation reaction of furosemide (5-(aminosulfonyl)-4-chloro-2-((furanylmethyl)amino)benzoic acid, dissolved in ethanol, with FeCl3 and the surfactant dodecyltrimethylammonium bromide (DTAB) in aqueous solution, yielding a colored compound on the surface of a filter paper. The reagent concentrations were optimized using a chemometric experimental design. The reflectometric measurements of the complex formed were carried out at 477nm. The linear range obtained was 1.65-9.00×10-3molL-1 of furosemide (R=0.997), and the detection and quantification limits were 4.9×10-4 and 1.62×10-3molL-1, respectively. The proposed method was successfully applied in the analysis of furosemide in spiked urine, demonstrating that it is a reliable alternative method for the detection of furosemide doping in sport. © 2012 Elsevier B.V..

Etanol: impactos sócio-ambientais de uma commodity em ascensão

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Plant growth and leaf-spot severity on eucalypt at different CO2 concentrations in the air

O objetivo deste trabalho foi avaliar os efeitos do aumento da concentração de CO2 do ar sobre o crescimento de plantas e sobre a mancha foliar causada por Cylindrocladium candelabrum em Eucalyptus urophylla. As mudas foram cultivadas durante 30 dias, a 451, 645, 904, 1.147 µmol mol-1 de CO2 ; em seguida, elas foram inoculadas com o patógeno e mantidas nas mesmas condições por sete dias. O aumento da concentração de CO2 aumentou a altura de plantas e a massa de matéria seca da parte aérea, e diminuiu a incidência e a severidade da doença. O diâmetro do caule não foi afetado pelos tratamentos. O aumento das concentrações de CO2 atmosférico afeta favoravelmente o crescimento de plântulas de eucalipto e reduz a severidade da mancha foliar.