A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

A novel indicator reaction for the catalytic determination of V(V) at ppb levels by the kinetic spectrophotometric method

A novel sensitive and relatively selective kinetic method is presented for the determination of V(V), based on its catalytic effect on the oxidation reaction of Ponceau Xylydine by potassium bromate in presence of 5-sulfosalicylic acid (SSA) as activator. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of Ponceau Xylydine at 640 nm between 0.5 to 7 min (the fixed time method) in H3PO4 medium at 25ºC. The effect of various parameters such as concentrations of H3PO4, SSA, bromate and Ponceau Xylydine, temperature and ionic strength on the rate of net reaction were studied. The method is free from most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (1-15 ng mL−1) with a detection limit of 0.46 ng mL-1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.8% (for ten replicate measurement at 95% confidence level). The proposed method suffers few interferences such as Cr(VI) and Hg(II) ions. The method was successfully applied to the determination of V(V) in tap water, drinking water, bottled mineral water samples and a certified standard reference material such as SRM-1640 with satisfactory results. The vanadium contents of water samples were also determined by FAAS for a comparison. The recovery of spiked vanadium(V) was found to be quantitative and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.

Determination of patulin in apple juice by HPLC using a simple and fast sample preparation method

The goal of this work was to develop a simple and rapid preparation method for patulin analysis in apple juice without previous clean-up. This method combined sonication and liquid extraction techniques and was used for determination of patulin in 37 commercial apple juices available on the market in the South of Brazil. The method performance characteristics were determined using a sample obtained in a local market fortified at five concentration levels of patulin and done in triplicates. The coefficient of variation for repeatability at the fortification level of 20.70µg.L-1 was 3.53 % and the recovery 94.63 %, respectively. The correlation coefficient was 0.9996 and agrees with the requirements for a linear analytical method value. The detection limit was 0.21µg.L-1 and the quantification limit 0.70 µg.L-1. Only three of the analyzed samples were upper the allowed level of 50.00 µg.L-1 recommended for the World Health Organization.

A simple spectrophotometric method for the determination of captopril in pharmaceutical preparations using ammonium molybdate

A simple, rapid and sensitive spectrophotometric method for the determination of captopril (CPT) in pharmaceutical formulations is proposed. This method is based on the reduction reaction of ammonium molybdate, in the presence of sulphuric acid, for the group thiol of CPT, producing a green compound (λ max 407 nm). Beer's law is obeyed in a concentration range of 4.60 x 10-4 - 1.84 x 10-3 mol l-1 of CPT with an excellent correlation coefficient (r = 0.9995). The limit of detection and limit of quantification were 7.31 x 10-6 e 2.43 x 10-5 mol l-1 of CPT, respectively. The proposed method was successfully applied to the determination of CPT in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the official reported method at 95 % confidence level.

A simple spectrophotometric method for the determination of tetracycline and doxycycline in pharmaceutical formulations using chloramine-T

A simple, rapid, accurate and inexpensive spectrophotometric method for the determination of tetracycline and doxycycline has been developed. The method is based on the reaction between these drugs and chloramine-T in alkaline medium producing red color products with absorbance maximum at the Λ = 535 and 525 nm for the tetracycline and doxycycline, respectively. The best conditions for the reactions have been found using multivariate method. Beer´s law is obeyed in a concentration ranges 1.03 x 10-5 to 3.61 x 10-4 mol L-1 and 1.75 x 10-5 to 3.48 x 10-4 mol L-1 for the tetracycline and doxycycline, respectively. The quantification limits were 5.63 x 10-6 mol L-1 and 7.12 x 10-7 mol L-1 for the tetracycline and doxycycline, respectively. The proposed method was successfully applied to the determination of these drugs in pharmaceutical formulations and the results obtained were in good agreement with those obtained by the comparative method at the 95% confidence level.

Nutritional status of Eucalyptus grandis clones evaluated by critical level and DRIS methods

Nutritional status of eight 1.0 and 4.7 years old clones of Eucalyptus grandis, cultivated in a medium textured Ustults - US - and a Quartzipsamments - PS - soils, in Lençóis Paulista, São Paulo, were evaluated by the Diagnosis and Recommendation Integrated System (DRIS) and Critical Level (CL) methods. Based on multivariate discriminant analysis, the DRIS indices described the nutritional status of trees better in relation to tree age and soil type than in relation to nutrient composition. Spearman's correlation coefficients showed statistically significant relationships between volumetric tree growth and nutrients when applying DRIS indices or foliar nutrient concentrations. However, the DRIS indices indicated a lower number of trees with nutritional deficiencies, in relation to the CL method. According to the CL method, P, S, and Ca were deficient in the majority of the soils and tree age categories. By the DRIS method, Ca was the only deficient nutrient in PS soils, and appeared to be particularly limited in one-year-old trees. In conclusion, the DRIS method was more efficient than the CL method in evaluating the nutritional status of eucalyptus trees.

Accuracy and efficiency evaluation of point-centered quarter method variations for vegetation sampling in an araucaria forest

In order to verify Point-Centered Quarter Method (PCQM) accuracy and efficiency, using different numbers of individuals by per sampled area, in 28 quarter points in an Araucaria forest, southern Paraná, Brazil. Three variations of the PCQM were used for comparison associated to the number of sampled individual trees: standard PCQM (SD-PCQM), with four sampled individuals by point (one in each quarter), second measured (VAR1-PCQM), with eight sampled individuals by point (two in each quarter), and third measuring (VAR2-PCQM), with 16 sampled individuals by points (four in each quarter). Thirty-one species of trees were recorded by the SD-PCQM method, 48 by VAR1-PCQM and 60 by VAR2-PCQM. The level of exhaustiveness of the vegetation census and diversity index showed an increasing number of individuals considered by quadrant, indicating that VAR2-PCQM was the most accurate and efficient method when compared with VAR1-PCQM and SD-PCQM.

Efficiency of distinct data mining algorithms for classifying stress level in piglets from their vocalization

Among the challenges of pig farming in today's competitive market, there is factor of the product traceability that ensures, among many points, animal welfare. Vocalization is a valuable tool to identify situations of stress in pigs, and it can be used in welfare records for traceability. The objective of this work was to identify stress in piglets using vocalization, calling this stress on three levels: no stress, moderate stress, and acute stress. An experiment was conducted on a commercial farm in the municipality of Holambra, São Paulo State , where vocalizations of twenty piglets were recorded during the castration procedure, and separated into two groups: without anesthesia and local anesthesia with lidocaine base. For the recording of acoustic signals, a unidirectional microphone was connected to a digital recorder, in which signals were digitized at a frequency of 44,100 Hz. For evaluation of sound signals, Praat® software was used, and different data mining algorithms were applied using Weka® software. The selection of attributes improved model accuracy, and the best attribute selection was used by applying Wrapper method, while the best classification algorithms were the k-NN and Naive Bayes. According to the results, it was possible to classify the level of stress in pigs through their vocalization.

Validation study of an overall radiation balance estimation method under Ponta Grossa (PR) Brazil weather conditions

Radiation balance is the fraction of incident solar radiation upon earth surface which is available to be used in several natural processes, such as biological metabolism, water loss by vegetated surfaces, variation of temperature in farming systems and organic decomposition. The present study aimed to assess and validate the performance of two estimation models for Rn in Ponta Grossa city, Paraná State, Brazil. To this end, during the period of 04/01/2008 to 04/30/2011, from radiometric data collected by an automatic weather station set at the Experimental Station, of the State University of Ponta Grossa. We performed a linear regression study by confrontation between measurements made through radiometric balance and Rn estimates obtained from Brunt classical method, and the proposed method. Both models showed excellent performance and were confirmed by the statistical parameters applied. However, the alternative method has the advantage of requiring only global solar radiation values, temperature, and relative humidity.

Comparison of Two- and Three-dimensional Ultrasonography in the Evaluation of Lesion Level in Fetuses with Spina Bifida

Purpose To evaluate the precision of both two- and three-dimensional ultrasonography in determining vertebral lesion level (the first open vertebra) in patients with spina bifida. Methods This was a prospective longitudinal study comprising of fetuses with open spina bifida who were treated in the fetal medicine division of the department of obstetrics of Hospital das Clínicas of the Universidade de São Paulo between 2004 and 2013. Vertebral lesion level was established by using both two- and three-dimensional ultrasonography in 50 fetuses (two examiners in each method). The lesion level in the neonatal period was established by radiological assessment of the spine. All pregnancies were followed in our hospital prenatally, and delivery was scheduled to allow immediate postnatal surgical correction. Results Two-dimensional sonography precisely estimated the spina bifida level in 53% of the cases. The estimate error was within one vertebra in 80% of the cases, in up to two vertebrae in 89%, and in up to three vertebrae in 100%, showing a good interobserver agreement. Three-dimensional ultrasonography precisely estimated the lesion level in 50% of the cases. The estimate error was within one vertebra in 82% of the cases, in up to two vertebrae in 90%, and in up to three vertebrae in 100%, also showing good interobserver agreement. Whenever an estimate error was observed, both two- and three-dimensional ultrasonography scans tended to underestimate the true lesion level (55.3% and 62% of the cases, respectively). Conclusions No relevant difference in diagnostic performance was observed between the two- and three-dimensional ultrasonography. The use of three-dimensional ultrasonography showed no additional benefit in diagnosing the lesion level in the fetuses with spina bifida. Errors in both methods showed a tendency to underestimate lesion level.

The Shadow Moiré method using the phase shifting technique and digital image processing: computational implementation and application to the 3D-reconstruction of a buckled plate

The Shadow Moiré fringe patterns are level lines of equal depth generated by interference between a master grid and its shadow projected on the surface. In simplistic approach, the minimum error is about the order of the master grid pitch, that is, always larger than 0,1 mm, resulting in an experimental technique of low precision. The use of a phase shift increases the accuracy of the Shadow Moiré technique. The current work uses the phase shifting method to determine the surfaces three-dimensional shape using isothamic fringe patterns and digital image processing. The current study presents the method and applies it to images obtained by simulation for error evaluation, as well as to a buckled plate, obtaining excellent results. The method hands itself particularly useful to decrease the errors in the interpretation of the Moiré fringes that can adversely affect the calculations of displacements in pieces containing many concave and convex regions in relatively small areas.

The application of Process Management for reliability enhancement of the Taguchi method

The concept of Process Management has been used by managers and consultants that search for the improvement of both operational or managerial industrial processes. Its strength is in focusing on the external client and on the optimization of the internal process in order to fulfill their needs. By the time the needs of internal clients are being sought, a set of improvements takes place. The Taguchi method, because of its claim for knowledge share between design engineers and people engaged in the process, is a candidate for process management implementation. The objective of this paper is to propose that kind of application aiming for improvements related with reliability of results revealed by the robust design of Taguchi method.

Comparison of anaerobic threshold determined by visual and mathematical methods in healthy women

Several methods are used to estimate anaerobic threshold (AT) during exercise. The aim of the present study was to compare AT obtained by a graphic visual method for the estimate of ventilatory and metabolic variables (gold standard), to a bi-segmental linear regression mathematical model of Hinkley's algorithm applied to heart rate (HR) and carbon dioxide output (VCO2) data. Thirteen young (24 ± 2.63 years old) and 16 postmenopausal (57 ± 4.79 years old) healthy and sedentary women were submitted to a continuous ergospirometric incremental test on an electromagnetic braking cycloergometer with 10 to 20 W/min increases until physical exhaustion. The ventilatory variables were recorded breath-to-breath and HR was obtained beat-to-beat over real time. Data were analyzed by the nonparametric Friedman test and Spearman correlation test with the level of significance set at 5%. Power output (W), HR (bpm), oxygen uptake (VO2; mL kg-1 min-1), VO2 (mL/min), VCO2 (mL/min), and minute ventilation (VE; L/min) data observed at the AT level were similar for both methods and groups studied (P > 0.05). The VO2 (mL kg-1 min-1) data showed significant correlation (P < 0.05) between the gold standard method and the mathematical model when applied to HR (r s = 0.75) and VCO2 (r s = 0.78) data for the subjects as a whole (N = 29). The proposed mathematical method for the detection of changes in response patterns of VCO2 and HR was adequate and promising for AT detection in young and middle-aged women, representing a semi-automatic, non-invasive and objective AT measurement.

The effects of stretching on the flexibility, muscle performance and functionality of institutionalized older women

Stretching has been widely used to increase the range of motion. We assessed the effects of a stretching program on muscle-tendon length, flexibility, torque, and activities of daily living of institutionalized older women. Inclusion/exclusion criteria were according to Mini-Mental State Examination (MMSE) (>13), Barthel Index (>13) and Lysholm Scoring Scale (>84). Seventeen 67 ± 9 year-old elderly women from a nursing home were divided into 2 groups at random: the control group (CG, N = 9) participated in enjoyable cultural activities; the stretching group (SG, N = 8) performed active stretching of hamstrings, 4 bouts of 1 min each. Both groups were supervised three times per week over a period of 8 weeks. Peak torque was assessed by an isokinetic method. Both groups were evaluated by a photogrammetric method to assess muscle-tendon length of uni- and biarticular hip flexors and hamstring flexibility. All measurements were analyzed before and after 8 weeks by two-way ANOVA with the level of significance set at 5%. Hamstring flexibility increased by 30% in the SG group compared to pre-training (76.5 ± 13.0° vs 59.5 ± 9.0°, P = 0.0002) and by 9.2% compared to the CG group (76.5 ± 13.0° vs 64.0 ± 12.0°, P = 0.0018). Muscle-tendon lengths of hip biarticular flexor muscles (124 ± 6.8° vs 118.3 ± 7.6°, 5.0 ± 7.0%, P = 0.031) and eccentric knee extensor peak torque were decreased in the CG group compared to pre-test values (-49.4 ± 16.8 vs -60.5 ± 18.9 Nm, -15.7 ± 20%, P = 0.048). The stretching program was sufficient to increase hamstring flexibility and a lack of stretching can cause reduction of muscle performance.

Tumor growth reduction is regulated at the gene level in Walker 256 tumor-bearing rats supplemented with fish oil rich in EPA and DHA

We investigated the effect of fish oil (FO) supplementation on tumor growth, cyclooxygenase 2 (COX-2), peroxisome proliferator-activated receptor gamma (PPARγ), and RelA gene and protein expression in Walker 256 tumor-bearing rats. Male Wistar rats (70 days old) were fed with regular chow (group W) or chow supplemented with 1 g/kg body weight FO daily (group WFO) until they reached 100 days of age. Both groups were then inoculated with a suspension of Walker 256 ascitic tumor cells (3×107 cells/mL). After 14 days the rats were killed, total RNA was isolated from the tumor tissue, and relative mRNA expression was measured using the 2-ΔΔCT method. FO significantly decreased tumor growth (W=13.18±1.58 vsWFO=5.40±0.88 g, P<0.05). FO supplementation also resulted in a significant decrease in COX-2 (W=100.1±1.62 vsWFO=59.39±5.53, P<0.001) and PPARγ (W=100.4±1.04vs WFO=88.22±1.46, P<0.05) protein expression. Relative mRNA expression was W=1.06±0.022 vsWFO=0.31±0.04 (P<0.001) for COX-2, W=1.08±0.02vs WFO=0.52±0.08 (P<0.001) for PPARγ, and W=1.04±0.02 vs WFO=0.82±0.04 (P<0.05) for RelA. FO reduced tumor growth by attenuating inflammatory gene expression associated with carcinogenesis.