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Decision Limit (decision + limit)
Selected AbstractsCombination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urineJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 6 2005Christof Van Poucke Abstract For the detection of anabolic steroid residues in bovine urine, a highly sensitive liquid chromatographic/electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method was developed using both positive and negative ionization. For four compounds the ESI mode was not sensitive enough and gas chromatographic/mass spectrometric GC/MS detection was therefore still necessary as a complementary method. The sample clean-up consisted of solid-phase extraction (SPE) on a C18 column followed by enzymatic hydrolysis and a second solid-phase extraction on a combination of a C18 and a NH2 column. After this last SPE clean-up, the eluate was split into two equal aliquots. One aliquot was further purified and after derivatization used for GC/MS analysis. The other aliquot was analyzed with LC/MS/MS in both ESI+ and ESI, modes. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CC,) were between 0.16 and 1 ng ml,1 for the compounds detected with the LC/MS/MS method. The developed method is used in routine analysis in our laboratory. Copyright © 2005 John Wiley & Sons, Ltd. [source] Development and validation of an HPLC confirmatory method for the determination of seven tetracycline antibiotics residues in milk according to the European Union Decision 2002/657/ECJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15 2007Victoria F. Samanidou Abstract An HPLC method with diode-array detection, at 355 nm, was developed and validated for the determination of seven tetracyclines (TCs) in milk: minocycline (MNC), TC, oxytetracycline (OTC), methacycline (MTC), demeclocycline (DMC), chlortetracycline (CTC), and doxycycline (DC). Oxalate buffer (pH 4) was used with 20% TCA as a deproteinization agent for the extraction of analytes from milk followed by SPE. The separation was achieved on an Inertsil ODS-3, 5 ,m, 250×4 mm2 analytical column at ambient temperature. The mobile phase, a mixture of A: 0.01 M oxalic acid and B: CH3CN, was delivered using a gradient program. The procedure was validated according to the European Union decision 2002/657/EC determining selectivity, stability, decision limit, detection capability, accuracy, and precision. Mean recoveries of TCs from spiked milk samples (50, 100, and 200 ng/g) were 93.8,100.9% for MNC, 96.8,103.7% for OTC, 96.3,101.8% for TC, 99.4,107.2% for DMC, 99.4,102.9% for CTC, 96.3,102.7% for MTC, and 94.6,102.1% for DC. All RSD values were lower than 8.5%. The decision limits CCa calculated by spiking 20 blank milk samples at MRL (100 ,g/kg) ranged from 101.25 to 105.84 ,g/kg, while detection capability CCbfrom 103.94 to 108.88 ,g/kg. [source] Monitoring of nosocomial invasive aspergillosis and early evidence of an outbreak using cumulative sum tests (CUSUM)CLINICAL MICROBIOLOGY AND INFECTION, Issue 9 2010J. Menotti Clin Microbiol Infect 2010; 16: 1368,1374 Abstract In order to provide a statistically based evaluation of the incidence of invasive aspergillosis (IA) over time, we applied the cumulative sums (CUSUM) methodology, which was developed for quality control and has already been applied for the surveillance of hospital-acquired infections. Cases of IA were recorded during a 5-year period. Incidence rates of cases assumed to be hospital-acquired, i.e. nosocomial IA (NIA), were analysed using CUSUM tests. Relationships between NIA, fungal contamination and construction or renovation work were tested using time-series methods. Between January 2002 and December 2006, 81 cases of NIA were recorded. CUSUM analysis of NIA incidence showed no significant deviation from the expected monthly number of cases until August 2005, and then the CUSUM crossed the decision limit, i.e. identified a significant increase in NIA as compared with the reference period (January 2002 to December 2004). Up to April 2006, the learning-curve CUSUM stayed over its limit, supporting an ongoing outbreak involving 24 patients, and then it significantly decreased in May 2006. Follow-up after May 2006 indicated no out-of-control situation, supporting a return to the baseline situation. In haematology wards, significant links were found between NIA incidence and fungal contamination of several sites at each ward (mainly unprotected common sites). An environmental source of contamination could be suspected, but no significant relationship was found between NIA incidence and ongoing construction or renovation. In conclusion, the CUSUM test proved to be well suited for real-time monitoring of NIA and for early identification and follow-up of an outbreak. [source] Performance characteristics according to Commission Decision 2002/657/EC in the fluorimetric determination of tetracycline in the absence and in the presence of magnesiumLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 6 2007Noelia Rodríguez Abstract The fluorimetric determination of tetracycline is usually carried out in the presence of some metals that, through the formation of a complex with this antibiotic, enhance its fluorescence emission, giving more sensitive determination methods. It is well established that magnesium is one of these metals. However, it is possible that higher signals do not mean a real improvement in the quality of the analytical method. In this work, the univariate and multivariate fluorescence determination of tetracycline is performed in the presence and absence of Mg2+, comparing the quality of the analyses through some performance characteristics that, according to Commission Decision 2002/657/EC define the functional qualities of analytical methods. The methods with the best performance characteristics were multivariate determinations carried out in the absence of Mg2+, both when emission or excitation spectra were taken, the decision limits (CC,) being 13.1 and 20.1 µg/L and the detection capabilities (CC,) 25.3 and 38.5 µg/L, respectively. This study points out through a case study that higher analytical signals do not necessarily mean better performance characteristics of a method of analysis. Copyright © 2007 John Wiley & Sons, Ltd. [source] | ||||||||||