This study determined the levels of total mercury in Spanish samples of baby food, fast food, and daily meal, which people of different ages consume, to evaluate potential toxicological risks through the contribution to the tolerable daily intake (TDI). The total mercury concentrations were determined in thirteen commercial baby foods for infants 6 to 12 months old, six types of fast foods prepared for children, and nine canteen menus prepared for adults. Samples were analyzed using a direct mercury analyzer, and the following concentration ranges were found: baby food (0.57-41.9 µg kg-1), fast food (0.54-68 µg kg-1), and adult menus (0.43-638 µg kg-1). The recovery of different amounts of spiked mercury ranged from 98.6 to 104.9%, and the method’s accuracy was checked with an analysis of different certified reference materials. The limits of detection and quantification obtained were 0.1 and 0.3 µg kg-1, respectively, with a relative standard deviation of up to 11%. The contribution of the samples to the TDI varied as follows: baby food (0.3-28%), fast food (0.5-102%), and adult menus (0.3-396%). Therefore, it was concluded that total mercury daily intake does not pose risks for Spanish children and adults if tuna is not included on their menu.

Abstract: A hard cap espresso machine was employed for the extraction of polyphenolic compounds from food samples as dry legumes and pulses. 100 mg of ground dry sample was mixed with a dispersing agent and placed in a refillable stainless steel capsule with a borosilicate filter. A complete polyphenol extraction was achieved by using 150 mL ethanol 50 % (v/v) in water and determined by Folin-Ciocalteu spectrophotometric method. The method provided a limit of detection of 0.4 mg g-1. The whole extraction procedure was achieved in less than one minute using the mild extraction conditions of 72°C and 19 bars given by the domestic machine. Fifteen varieties of food samples (3 lentils, 6 beans, 5 chickpeas, and 1 sorghum) were purchased in Spanish and Tunisian markets and analyzed by the proposed procedure. Obtained results were compared with those found by a reference extraction method based on ultrasound-assisted extraction, being statistically comparable. The content of polyphenolic compounds in the analyzed commercial samples varied from 4.6 to 5.5 mg g-1 for lentils, from 3.4 to 5.8 mg g-1 for beans, from 2.2 to 3.5 mg g-1 for chickpeas, and 3.0 mg g-1 for sorghum.

Resumen: En este estudio se evalúa el empleo de una cafetera expreso para la extracción de polifenoles en legumbres. La muestra (100 mg) triturada y seca se mezcla con un agente dispersante en el interior de una capsula de acero inoxidable reutilizable junto con un filtro de borosilicato. La extracción cuantitativa de los polifenoles de la muestra se consigue con 150 mL de etanol al 50 % (v/v) en agua, realizando la determinación por el método espectrofotométrico de Folin-Ciocalteu, obteniendo un límite de detección de 0.4 mg g-1. La extracción se realiza en menos de un minuto en las condiciones suaves de 72°C y 19 bares, proporcionadas por la cafetera. En este estudio 15 muestras de legumbres (3 lentejas, 6 judías, 5 garbanzos, y 1 sorgo) se adquirieron en mercado locales de España y Túnez, y se analizaron por el procedimiento propuesto, comparando los resultados obtenidos con un método de referencia basado en la extracción asistida por ultrasonidos, siendo estadísticamente comparables. El contenido total de polifenoles en las muestras analizadas varió entre de 4.6 a 5.5 mg g-1 para lentejas, de 3.4 a 5.7 mg g-1 para judías, de 2.2 a 3.5 mg g-1 para garbanzos, y 3.0 mg g-1 para sorgo.

Resumen El pez león (Pterois volitans) invadió la región del Caribe y tiene el potencial de alterar la composición y estructura de las comunidades de peces en los arrecifes coralinos. El objetivo de este estudio fue analizar los índices de diversidad en las comunidades de peces nativos en sitios invadidos por el pez león en dos áreas marinas protegidas (AMP) del Caribe y compararlos con datos previos a la invasión. En ambas AMP, Parque Nacional Guanahacabibes (PNG) en el occidente de Cuba y Parque Nacional Arrecifes de Xcalak (PNAX) en el S de Quintana Roo, se realizaron censos visuales de las especies de peces en hábitats durante las épocas de seca y lluvia del 2013-2015. Se evaluaron nueve sitios, mediante conteos estacionarios. Se registró mayor riqueza de especies en el PNG (43.47±5.14) que en el PNAX (40.22±4.96). No se observaron diferencias entre épocas en ninguna de las AMP. El pez león se ubicó entre las especies más abundantes del PNG. La abundancia media en el PNG (0.76 ± 1.25) fue mayor a la registrada en el PNAX (0.19±0.46). La diversidad disminuyó después de la llegada del pez león en un solo sitio del PNG y en dos sitios del PNAX, pero al parecer estos resultados están más asociados al efecto de la pesca que a la presencia del pez león. A partir de los resultados y asumiendo que los cambios en las comunidades de peces por el pez león podrían no detectarse aún, recomendamos seguir los monitoreos de los descriptores comunitarios para detectar cambios futuros en las comunidades de peces.

Abstract Lionfish (Pterois volitans) invaded the Caribbean region with the potential to alter the composition and structure of native coral reef fish communities. The objective of this study was to analyze the diversity indices of these fish communities potentially affected by lionfish predation and to compare with pre-invasion data. The study was undertaken in two Caribbean marine protected areas (MPAs): Guanahacabibes National Park (PNG) in W Cuba and Xcalak Reefs National Park (PNAX) in S Quintana Roo. We carried out visual censuses of fish species in reef habitats during the dry and rainy seasons of the period 2013-2015. For this, nine sites were defined and evaluated using stationary counts. Our results showed higher species richness (43.47 ± 5.14) and mean abundance (0.76 ± 1.25) in PNG than in PNAX (40.22 ± 4.96, 0.19 ± 0.46, respectively). Diversity decreased after the arrival of lionfish in a single site of PNG and in two sites of the PNAX, but apparently, these results are more related to the fishing activity effect than to the lionfish presence. Based on the results and assuming that changes in the native fish communities by lionfish may not yet be detected, we recommend to continue the monitoring community descriptions in order to detect future changes in native fish communities. Rev. Biol. Trop. 66(1): 189-203. Epub 2018 March 01.

Neste trabalho foi desenvolvido um sistema não cromatográfico rápido, sensível e simples para a determinação de Sb(III), Sb(V), Te(IV) e Te(VI) em amostras de cereais. O procedimento baseia-se na extração assistida por ultra-som e na determinação por espectrometria de fluorescência atômica acoplada com geração de hidretos (HG AFS). Foram realizados estudos preliminares com o intuito de avaliar a eficiência da extração usando 1 mol L-1 ácido fosfórico, 1 mol L-1 ácido nítrico, água regia, 1 mol L-1 ácido sulfúrico e 6 mol L-1 ácido clorídrico. A extração com água régia apresentou uma evidente interconversão das espécies durante o processo. No entanto, o H2SO4 apresentou-se como o melhor agente de extração com eficiências maiores do que 90% em relação ao conteúdo total de Sb e Te (ambos os elementos foram previamente quantificados), não apresentando interconversão nenhuma. Estudos de recuperação para diferentes níveis de adição das espécies comprovaram a não interconversão das espécies. O método forneceu limites de detecção na faixa de 0,1 a 1,0 ng g-1 com desvios padrão relativos de 5,4-9,2% para 10 análises independentes de amostras que continham baixas concentrações de espécies de Sb e Te.

A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L-1 phosphoric acid, 1 mol L-1 nitric acid, aqua regia, 1 mol L-1 sulfuric acid and 6 mol L-1 hydrochloric acid. The extraction with aquaregia showed a clear interconversion of the species during the process, being H2SO4 the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g-1 with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species.

Objectives: Our goal is to analyze the degree of concordance between the Gleason score (GS) obtained in prostate biopsies and the one after radical prostatectomy. The intention is to know whether 12-core biopsy, instead of 6 (sextant biopsy), improves, or not, this correlation. Methods: A Cohort/prevalence study was conducted on 128 patients who underwent prostate biopsy and subsequent radical prostatectomy. Patients showing biopsy Gleason values greater or equal to 6 were selected as candidates for radical prostatectomy. Results: Mean age of the group of 128 patients was 62.9 years, with a mean PSA value of 8.53ng/ml. There was concordance between biopsy Gleason score and that obtained after radical prostatectomy in 63.28% of cases, while discordance was found in 36.72% of cases. There were not significant statistical differences after comparing results obtained between Gleason score concordance after 6 or 12-core biopsies and that obtained after radical prostatectomy. Conclusions: We have noticed a low correlation between Gleason score after biopsy when it was com-pared with that obtained after radical prostatectomy, while these results are similar to those found in the literature. We did not find better results regarding Gleason score correlation after biopsies performed with 12 cores instead of 6.

Objetivo: El cáncer de próstata es una patología cada vez más prevalente por la longevidad de la población. Es por ello que cada vez con más frecuencia se somete a los pacientes a realización de biopsia prostática para realizar su diagnóstico de certeza. Nuestro objetivo fue analizar la relación del score gleason obtenido en la biopsia de próstata con el obtenido tras prostatectomía radical. Se pretendió analizar si la obtención de 12 cilindros en lugar de 6 (biopsia sextante) mejora o no esta relación. Métodos: Se realizó un estudio de casos y controles con 128 pacientes (98 casos en los que se obtuvó 6 cilindros y 30 controles en los que se obtuvieron 12 cilindros) que fueron sometidos a biopsia de próstata y posterior prostatectomía radical. Para ello se seleccionaron a pacientes con Gleason biópsico mayor o igual de 6 y candidatos a prostatectomía radical. Resultados: La media de edad de los 128 pacientes incluidos en el estudio fue de 62,9 años, con una media de PSA de 8,53 ng/ml. Se observó igualdad de Score Gleason biopsia/prostatectomía en el 63,28 % de los pacientes y desigualdad en el 36,72 %. Tras comparar los resultados obtenidos entre la relación del score gleason tras extracción de 6 o 12 cilindros y tras prostatectomía radical no se apreciaron diferencias estadísticamente significativas Conclusiones: La correlación gleason biopsia-prostatectomía radical es baja. No apreciamos mejoría significativa para esta correlación el obtener 12 cilindros en lugar de 6.

Objectives: The relationship between hyperparathyroidism and lithiasis is quite known, so the study of parathyroid glands is especially mandatory in the face of relapses. Our objective is to analyze both primary hyperparathyroidism (PHPT) associated with renal lithiasis and the evolution of this condition after parathyroidectomy, as well as to study factors associated with the presence of lithiasis or bone pathology, and carry out a review on bibliography. Methods: We describe a retrospective study of a series comprising 287 cases of hyperparathyroidism: 237 of them were primary and the remaining 50, secondary. We have included: sex, age, evolution time and symptoms, diagnostic tests (biochemical, radiological and histological). Factors such as number of episodes prior to diagnosis and treatments were analyzed in patients with symptomatic lithiasis to know whether patients exhibited residual lithiasis after the management of calculi or whether patients underwent episodes after parathyroidectomy, or whether or not they were treated. Statistical analysis was carried out through SPSS 15.0 for Windows. Results: Forty five percent of the patients had suffered lithiasis episodes; 50%, osteopenia/osteoporosis; 23%, musculoskeletal pain; 23%, asthenia and/or depressive syndrome. In 13.5% of cases, diagnosis was supported by the presence of hypercalcemia; no other symptoms were detected. We have analyzed factors that favor or inhibit renal lithiasis formation and compared biochemical parameters from the group of primary hyperthyroidism that exhibited lithiasis (41 patients) with those patients who did not (49). We noted that lithiasis patients showed higher values of calcium, alkaline phosphatase, intact PTH, mean PTH, osteocalcin, and chlorine/phosphate, calciuria and phosphaturia indexes. Student's t test on two independent samples revealed significant statistical differences in calcium levels (p<0.05), intact PTH (<0.05) and osteocalcin. Conclusions: Primary hyperparathyroidism patients with lithiasis presented higher values of parathormone, alkaline phosphatase, osteocalcin, and Cl/P and calciuria indexes than lithiasis-free PHPT patients. These patients exhibit objective improvement of symptoms after parathyroidectomy, and rarely a recurrence of lithiasis, a factor that generally coincides with persistence of residual lithiasis.

Objetivo: La relación hiperparatiroidismo-litiasis renal es bien conocida y el estudio de paratiroides es obligado en paciente con litiasis, sobre todo si hay recidivas. Nuestro objetivo es analizar los casos de HPTP con litiasis renal y su evolución tras paratiroidectomía; estudiar los factores que se asocian a la presencia de litiasis o patología ósea y revisión bibliográfica. Métodos: Estudio descriptivo retrospectivo de una serie de 287 casos de hiperparatiroidismo: 237 primarios, 50 hiperparatiroidismos secundarios. Hemos analizado: sexo, edad, tiempo de evolución, clínica, pruebas diagnósticas (bioquímicas, radiológicas e histológicas). En pacientes con clínica de litiasis se ha analizado el número de episodios previos al diagnóstico y su tratamiento, si presentaban litiasis residual tras el tratamiento del cálculo, si sufrieron episodios posteriores a la paratiroidectomía y si fueron tratados o no. Análisis estadístico con SPSS 15.0 para Windows. Resultados: El 45% de pacientes había presentado episodios de litiasis, 50% osteopenia/osteoporosis, 23% algias osteomusculares, astenia y/o síndrome depresivo el 23%; en el 13,5% de los casos el diagnóstico se realiza tras el hallazgo de hipercalcemia sin otros síntomas. Analizamos factores favorecedores o inhibidores de formación de litiasis renal, hemos comparado parámetros bioquímicos del grupo de hiperparatiroidismos primarios con litiasis (41 pacientes) con grupo sin litiasis (49). Observamos que enfermos con litiasis presentan cifras más elevadas de calcio, fosfatasa alcalina, PTHi, PTHm, osteocalcina, índice cloro/fosfato, calciuria y fosfaturia. Al aplicar el test "t" Student para dos muestras independientes se encontraron diferencias estadísticamente significativas en niveles de calcio (p<0,05), PTHi (p<0,05) y osteocalcina. Conclusiones: Los casos de hiperparatiroidismo primario con litiasis presentan cifras de calcio, para-thormona, fosfatasa alcalina, osteocalcina, índice Cl/P y calciuria más elevadas que los pacientes con HPTP sin litiasis. Estos pacientes presentan mejoría objetiva de síntomas tras paratiroidectomía, es poco frecuente la recurrencia de litiasis, que generalmente coincide con la persistencia de litiasis residual

Objective: We describe one case of recurrent lithiasis associated with anatomical alteration of the renal pelvis related to previous surgery. Methods/Results: The patient presented a urinary tract infection episode, complicated with pyonephrosis and septicemia. In the intravenous urography, infectious radiopaque pyelocaliceal multiple and complex lithiasis can be seen, as well as kidney hydronephrosis grade III-IV. Important pyelic sclerosis secondary to previous surgery on the renal unit was seen. Nephrectomy was performed with lower pole nephrolithotomy and reconstruction of the upper urinary tract through ureterocalicostomy. Two and a half years after surgery, control urogram shows absence of urolithiasis and a slight delay of renal function. Conclusions: Ureterocalicostomy is indicated in cases of ureteropelvic junction obstruction associated with intrarenal pelvis caused by alterations of fusion, rotation or location of kidney. It is also indicated in cases of severe peripyelic fibrosis secondary to previous pyeloplasty failure or renal surgery. In our case, in addition to the infectious component of lithiasis, an anatomical alteration, probably secondary to previous surgery, caused the chronification of lithiasis. Facing such suspicion a surgical management was undertaken to eliminate the lithiasis and get a correct derivation of the working area of the kidney, in order to prevent further recurrences.

Objetivo: Presentamos un caso de litiasis recidivante asociado a alteración anatómica de la pelvis renal secundaria a cirugía. Métodos/Resultados: La paciente presenta un episodio de infección urinaria complicada con pionefrosis y septicemia. En la urografía intravenosa se observa litiasis radiodensa infecciosa, pielolocalicial múltiple compleja, sobre riñón con hidronefrosis grado III-IV por importante esclerosis piélica secundaria a cirugía previa sobre dicha unidad renal. Se realiza nefrectomía polar inferior con nefrolitotomía y reconstrucción de la vía urinaria superior mediante uréterocalicostomía. Dos años y medio después de la cirugía la urografía de control refleja ausencia de litiasis y leve retraso de la función renal. Conclusiones: La ureterocalicostomía está indicada en casos de obstrucción de la unión ureteropiélica asociada a una pelvis intrarrenal por alteraciones de la fusión, rotación o localización renal, y en casos de fibrosis peripiélica severa secundaria a una pieloplastía fallida o cirugía renal previa. En el caso presentado además del componente infeccioso de las litiasis, una alteración anatómica, probablemente secundaria a la cirugía previa, provocaba una perpetuación de la clínica litiásica. Ante tal sospecha se impuso una solución de tipo quirúrgico que solucionara en un tiempo tanto la eliminación de la litiasis como una correcta derivación de la zona funcionante del riñón para evitar recidivas posteriores.

Um procedimento para determinação de selênio em águas, completamente mecanizado, foi desenvolvido empregando um fotômetro baseado em LED e mini-bombas solenóide como dispositivos de propulsão. O método proposto é baseado na reação de selênio com iodeto de potássio em meio ácido para liberar iodo, o qual oxida a variamina azul formando um composto violeta que absorve em 530 nm. O sistema foi mecanizado empregando o processo de multicomutação em fluxo e uma estratégia de parada de fluxo na etapa final para desenvolvimento da reação. A curva analítica foi linear entre as concentrações de 0,010 a 0,500 mg L-1, segundo a equação ΔA = 0,501 (± 0,004) C (R = 0,999). O limite de detecção (3σ/S) obtido com o método proposto foi de 0,004 mg L-1. Desvios padrão relativo de 1,6 e 1,8% (n = 4) foram obtidos para soluções de Se com concentrações de 0,050 e 0,200 mg L-1, respectivamente. A freqüência de amostragem foi de 23 determinações por hora, e a exatidão foi de 95% de probabilidade.

It has been developed a fully mechanised procedure for the determination of selenium in waters employing a LED based spectrometer and solenoid multi-pumps as solution propelling devices. The proposed method is based on the reaction of selenium with potassium iodide in an acidic medium to liberate iodine, which oxidizes Variamine Blue to form a violet-colour species which absorb at 530 nm. The system was mechanised using the multicommutation process and a stopped flow strategy in the final step reaction. The analytical curve was linear between 0.010 and 0.500 mg L-1, with an equation ΔA = 0.501 (± 0.004) C and r = 0.999. The limit of detection (3σ/S) obtained for the proposed method was 0.004 mg L-1. The relative standard deviation for Se solutions of 0.050 and 0.200 mg L-1 (n = 4) were 1.6 and 1.8% respectively, the sampling throughput was 23 determinations per hour, and accuracy was 95% probability level.

Objectives: The use of laser for endoscopic lithotripsy started in 1968 when Mulvaney tried a ruby laser without success; Later on, the CO2 laser and the Nd: YAG were tried. With the pulsed dye and alexandrite lasers energetic performances between 30 and 200 mJ are obtained, their capacity of fragmentation is not universal and is limited to small stones, generally ureteral stones, so that it has not been a therapeutic alternative for bladder lithiasis. The holmium laser generates energy pulses of 400-2500mJ, it is able to fragment every type of stone. The objective of this work is to analyze the results of endoscopic bladder lithotripsy with holmium-YAG laser. Methods: In the period between 2006-2008 we treated 21 cases of bladder lithiasis, with a stone size between 1 and 4 cm in patients from 8-76 years, six women and 15 men, which correspond to: four cases of infantile lithiasis, 3 of uric acid, one case of cystine, seven cases of calcium oxalate and/or phosphate, five cases of bladder lithiasis growing around a double J catheter, and one case of lithiasis within an intravesical ureterocele. Treatment was performed with a 20W Dornier Medilas holmium-YAG equipment, applied using children/adult cystoscopes or 7-8.5 Ch ureteroscopes, both semirigid and flexible. Post operative control included KUB x-ray and ultrasound. We performed a study of lithogenic risk factors and stone fragments analysis. Results: The 21 cases described are all secondary or type II bladder lithiasis. In all cases the absence of residual lithiasis was checked with imaging studies and the lithogenic risk factors were corrected with medical or surgical procedures. Conclusions: We consider that today bladder endoscopic lithotripsy with holmium laser is a therapeutic alternative. Despite there are multiple options for endoscopic treatment, transurethral lithotripsy with holmium laser offers good results with a low complication rate.

Objetivo: El uso del láser para litotricia endoscópica, comienza en 1968 al utilizar Mulvaney un láser de rubí sin éxito, posteriormente se probaron láser de CO2 y Neodymio-YAG. Con el láser pulsado de colorante y el láser de alexandrita se obtienen unos rendimientos energéticos que oscilan de 30 a 200 mJ, su capacidad de fragmentación no es universal y esta limitada a pequeños cálculos, generalmente ureterales, por lo que no han sido alternativa terapéutica en la litiasis vesical. El láser de Holmio genera pulsos de energía de 400-2500 mJ, capaz de fragmentar todo tipo de cálculos. El Objetivo de este trabajo es analizar los resultados de la litotricia vesical endoscópica con láser de holmio YAG. Métodos: en el periodo de 2006-2008 hemos tratado 21 casos de litiasis vesical, con tamaños de 1 a 4 cm. en pacientes de 8-76 años, 6 mujeres y 15 hombres, que corresponden a: Cuatro casos de litiasis infantil, 3 de ácido úrico, 1 caso de cistina, litiasis de oxalato y/o fosfato cálcico en 7 casos, 5 casos de litiasis vesical sobre extremo inferior de doble jota, 1 caso de litiasis en ureterocele intravesical. El tratamiento se ha realizado con un equipo Dornier Medilas de 20 watios de Holmio-YAG como fuente de energía, que se ha aplicado a través de cistoscopios infantil-adulto o ureteroscopios de 7-8.5 Ch. semirrígido y flexible. El control post-operatorio se ha realizado con radiografía simple de aparato urinario y ecografía. Realizamos estudio de factores de riesgo litógeno y análisis de los fragmentos del cálculo. Resultados: Los 21 casos descritos corresponden a litiasis vesical secundaria o tipo II. En todos los casos se ha comprobado la ausencia de litiasis residual con estudios de imagen y se han corregido los factores de riesgo litógeno con procedimientos médicos o quirúrgicos. Conclusiones: Consideramos que hoy, la litotricia vesical endoscópica con láser de holmio si es alternativa terapéutica. A pesar de que existen múltiples opciones de tratamiento endoscópico, la litotricia transuretral con láser de holmio ofrece buenos resultados con un bajo porcentaje de complicaciones.

Um procedimento simples, rápido e preciso de cromatografia líquida de alta eficiência (HPLC) foi desenvolvido para a determinação de oxadiazona em formulações concentradas de pesticidas emulsificáveis. 20 µL de amostra, diluída em acetronitrila, foram injetados em uma coluna Kromasil C18 (250 × 4,6 mm, 5 µm), usando acetonitrila:água (80:20) como fase móvel, numa velocidade de fluxo de 1 mL min-1. Oxadiazona foi determinada por medidas de absorbância a 292 nm. Obteve-se, usando-se o procedimento desenvolvido, um limite teórico de detecção de 0,02 µg mL-1, um limite de quantificação de 0,047 µg mL-1, correspondendo a 0,02 e 0,07% m/v na amostra original e desvio padrão relativo de 0,08%, para três análises em replicata de amostras contendo 25% m/v de oxadiazona. A precisão do método foi evidenciada pelas porcentagens de recuperação de 98% a 99% para amostras contendo 0,015 a 0,085 mg de oxadiazona, assim como pela comparação entre os resultados encontrados pelo procedimento recomendado e pela espectrofotometria de infravermelho com transformada de Fourier (FTIR), para amostras reais de produtos formulados.

A simple, fast and precise high performance liquid chromatographic (HPLC) procedure has been developed for the determination of oxadiazon in emulsifiable concentrated pesticide formulations. 20 µL of diluted sample in acetonitrile were injected in a Kromasil C18 (250 ×am injetados em uma coluna Kromasil C18 4.6 mm, 5 µm) column, using acetonitrile:water (80:20) as mobile phase at 1 mL min-1 flow rate and oxadiazon determined by absorbance measurement at 292 nm. A theoretical limit of detection of 0.02 µg mL-1, a limit of quantification of 0.047 µg mL-1, corresponding to a 0.02 and 0.07% m/v in the original sample, and a relative standard deviation of 0.08% for three replicate analysis of samples containing 25% m/v. Oxadiazon were achieved using the developed procedure. The accuracy of the whole method was evidenced by recovery percentages from 98% to 99% for samples spiked with 0.015 to 0.085 mg oxadiazon as well as by the good comparability between results found by the recommended procedure and by Fourier Transform Infrared (FTIR) spectrophotometry for actual samples of formulated products.

Objectives: Current treatment of hypercalciuria is still controversial, not being recommended calcium restriction since it may cause a negative balance with important consequences to bone metabolism. In adults, the use of biphosphonates (sodium alendronate) has shown a good response. Biphosphonates are synthetic analogs of the endogenous pirophosphate. Pirophosphate is the simplest form of phosphate. In 1968, Fleisch demonstrated that inorganic pirophosphate inhibits the precipitation of calcium phosphate. The differences between various biphosphonates are in the safety margin between their inhibitor effect for bone resorption and the inhibitor effect for mineralization; bone resorption inhibition has been their most widely spread application. The objective of this work is to analyze the clinical and biochemical effect of biphosphonates in patients with hypercalciuria, osteopenia and renal lithiasis. Methods: From 1996 to 2006 we treated 25 cases of recurrent renal lithiasis associated with hypercalciuria and primary or secondary bone mass loss. All cases were treated with sodium alendronate and oral calcium (1000-1200 mg/day). We analyze tolerance and treatment compliance, side effects, biochemical effects on blood and urine, effect on bone mineralization, and the outcome of lithiasic disease before and after treatment. Results: All patients have followed the recommendations for the administration of the drug (sodium alendronate 10 mg/day or 70 mg/week), have had good tolerance without relevant side effects, and no one quit treatment. 76% of the cases have had remission of the lithogenesis activity and 24% reduction, and all cases have had an increase of bone mineralization. Conclusions: In this group of selected patients with recurrent lithiasis and osteopenia the treatment with biphosphonates alone or associated with thiazide diuretics has given good results in renal lithiasis control and bone demineralization. The extension of indications should be analyzed in a multicentric randomized study.

Objetivo: El tratamiento actual de la hipercalciuria aún es controvertido, no recomendándose la restricción de calcio ya que puede producir un balance negativo con importantes consecuencias en el metabolismo óseo. En adultos, el uso de bifosfonatos (alendronato sódico) ha mostrado buena respuesta. Los bifosfonatos son análogos sintéticos del pirofosfato endógeno, el pirofosfato es la forma más simple del fosfato, Fleisch en 1968 demostró que el pirofosfato inorgánico inhibe la precipitación del fosfato cálcico. La diferencia entre los diferentes bifosfonatos está en el margen de seguridad entre su efecto inhibidor de la resorción ósea y el efecto inhibidor de la mineralización, su aplicación más difundida ha sido como inhibidores de la resorción ósea. El objetivo de este trabajo, es analizar el efecto clínico y bioquímico de los bifosfonatos en enfermos con hipercalciuria, osteopenia y litiasis renal. Métodos: En el periodo de 1996-2006 hemos tratado 25 casos de litiasis renal recidivante asociada a hipercalciuria y perdida de masa ósea primaria o secundaria. En todos los casos se ha realizado tratamiento con alendronato sódico y aporte oral de calcio equivalente a 1000-1200 mg/día. Analizamos, tolerancia y adherencia al tratamiento, efectos secundarios, efectos bioquímicos en sangre y orina, efectos sobre mineralización ósea y evolución de la actividad litiásica antes y después del tratamiento. Resultados: Todos los pacientes han seguido las recomendaciones de administración del fármaco (alendronato sódico 10 md/día o 70 mg/semana), han manifestado buena tolerancia y no se han producido efectos secundarios relevantes ni abandonos del tratamiento. En el 76% de los casos se ha producido remisión de la actividad litógena y en el 24% se ha reducido la actividad litiásica, en todos los casos ha aumentado la mineralización ósea. Conclusiones: En este grupo seleccionado de pacientes con litiasis recidivante y osteopenia, el tratamiento con bifosfonatos solos o asociados a tiacidas ha obtenido buenos resultados en el control de la litiasis renal y desmineralización ósea. La ampliación de sus indicaciones debe analizarse en un estudio randomizado multicéntrico.

Um procedimento empregando detecção quiluminescente para determinação de carbaril em águas naturais utilizando acetilcolinesterase e colina oxidase é descrito. O módulo de análise projetado para implementar o processo de multicomutação controlado por microcomputador foi constituído por cinco válvulas solenóides, duas colunas com enzimas imobilizadas em esferas de vidro e cela de fluxo para detecção de quimiluminescência. Nas melhores condições experimentais foi obtida faixa linear entre 25 a 700 µg L-1 de carbaril. Amostras de água foram fortificadas com carbaril e as recuperações variaram entre 95 e 101%. Limite de detecção e coeficiente de variação foram estimados em 11 µg L-1 (99,7% nível de confiança) e 1,3% (n = 20), respectivamente. Outras características analíticas tais como freqüência de amostragem de 72 determinações por hora, consumo de reagente de 2,1 mg de hexacianoferrato de potássio(III) e 0,069 mg de luminol por determinação, também, foram obtidas.

A chemiluminescence procedure for the determination of carbaryl in natural waters using acetylcholinesterase and choline oxidase is described. The flow system designed to implement multicommutation approach controlled by microcomputer comprised five solenoid valves, two columns with immobilized enzymes on controlled pore glass beads and chemiluminometric flow cell. In the best experimental conditions a linear response ranging from 25 to 700 µg L-1 carbaryl was obtained. Water samples were spiked with carbaryl in order to access the accuracy and recoveries between 95 and 101% were obtained for a concentration level ranging from 25 to 100 µg L-1 carbaryl. Detection limit and variation coefficient were estimated as 11 µg L-1 (99.7% confidence level) and 1.3% (n = 20), respectively. Other profitable features such as a sample throughput of 72 determinations per hour, a reagent consumption of 2.1 mg potassium hexacyano ferrate(III) and 0.069 mg luminol per determination were also achieved.

Foi desenvolvido um método simples usando Infra-Vermelho com Transformada de Fourier (IRFT) para a determinação de Imidaclopride em formulações pesticidas. As amostram foram diluídas com CHCl3 e os espectros de IRFT de amostras e padrões foram obtidos numa resolução nominal de 4 cm-1, entre 4000 e 900 cm-1, com acumulação de 25 espectros. A determinação de Imidaclopride foi feita medindo-se tanto a área do sinal obtido entre 1577 e 1567 cm-1 ou a altura do sinal a 1572 cm-1, ambos com correção de linha base horizontal a 1900 cm-1. Os limites de detecção atingidos da ordem de 9 µg g-1, foram apropriados para a determinação de Imidoclopride em formulações comercias disponíveis. Os resultados com IRFT forma estatisticamente comparáveis àqueles encontrados para Cromatografia Líquida de Alta Performance (HPLC). O procedimento desenvolvido reduz o consumo de solventes orgânicos por preparação de amostra, de 53 mL de CH3CN requeridos com HPLC para 2,5 mL de CHCl3, reduzindo o descarte gerado, e aumenta a freqüência de medidas de 10 para 60 amostras h-1, quando comparado ao método de referência usando HPLC-UV.

A simple method has been developed for Fourier Transform Infrared (FTIR) determination of Imidacloprid in pesticide formulations. Samples were diluted with CHCl3 and the FTIR spectra of samples and standards were obtained at a nominal resolution of 4 cm-1 from 4000 to 900 cm-1 accumulating 25 scans. Imidacloprid determination was based on the measure of either peak area from 1577 to 1567 cm-1 or peak height at 1572 cm-1, both corrected using a horizontal baseline defined at 1900 cm-1. The limits of detection achieved, of the order of 9 µg g-1, were appropriate for the determination of Imidacloprid in commercially available formulations. FTIR results were statistically comparable to those found by High Performance Liquid Chromatography (HPLC). The procedure developed reduces organic solvent consumption, per sample preparation, from 53 mL CH3CN required for HPLC to 2.5 mL CHCl3, and reduces waste generation also increasing the sample measurement frequency from 10 h-1 to 60 h-1 as compared with the HPLC-UV reference method.