205 resultados para external validation


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This article describes the development of SPE and HPLC methods for the simultaneous determination of metformin and glipizide, gliclazide, glibenclamide or glimperide in plasma. Several extraction and HPLC methods have been described previously for the determination of each of these analytes in plasma separately. The simultaneous determination of these analytes is important for the routine monitoring of diabetic patients who take combination medications and for studying the pharmacokinetics of the combined dosage forms. In addition this developed method can serve as a standard method for the plasma determination of these analytes therefore saving time, effort and money. The recoveries of the developed methods were found to be between 76.3% and 101.9%. The limits of quantification were between 5 and 22.5 ng/ml. The intraday and interday precision (measured by coefficient of variation, CV%) was always less than 9%. The accuracy (measured by relative error %) was always less than 12%. Stability analysis showed that all analytes are stable for at least 3 months when stored at -70degreesC. (C) 2004 Elsevier B.V. All rights reserved.

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Concentrations of the coccidiostat nicarbazin as low as 2 mg/kg in feed can result in violative drug residues arising in poultry liver. A lateral flow device (LFD) was developed for the detection of contaminating concentrations of nicarbazin following solvent extraction of poultry feeds. Test results, as determined by both visual and instrumental measurement, are available within minutes. For 22 feed samples, nicarbazin-free and fortified at 2 mg/kg, the % relative inhibition ranged from 0 to 45% and from 53 to 85%, respectively. Nicarbazin contamination at the critical concentration (2 mg/kg) can be determined in all cases providing the sampling is representative. A wide range of feed samples taken at a mill that incorporated nicarbazin into poultry feed were analyzed. Data generated for these samples by both the LFDs and a mass spectrometric method were compared, and a significant correlation was achieved.

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The use of cortisol levels as a measure of stress is often complicated by the use of invasive techniques that may increase hypothalamic-pituitary-adrenal (HPA) axis activity during sample collection. The goal of this study was to collect samples noninvasively and validate an enzyme-immunoassay (EIA) for the measurement of cortisol in urine to quantify HPA axis activity in the bearded emperor tamarin (Saguinus imperator subgrisescens). Urine samples were collected from trained subjects between 0700 and 0730 hr during a 1-month period, and were pooled for immunological validation. We validated the assay immunologically by demonstrating specificity, accuracy, precision, and sensitivity. For biological validation of the assay, we showed that levels of urinary cortisol (in samples collected between 0700 and 1700 hr) varied significantly across the day. Cortisol concentration was lowest at 0700 hr, increased to a mid-morning peak (0900 hr), and declined across the remainder of the day in a typical mammalian circadian pattern. We thus demonstrate that urinary cortisol can be used to quantify HPA activity in S. i. subgrisescens. (C) 2004 Wiley-Liss, Inc.

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The effects of the external circuit on plasma instabilities in all inductive plasma source are investigated. The instabilities are found to be asymmetric with respect to the circuit input impedance. A simplified model of the antenna-plasnia coupling provides an explanation of the asymetry.