54 research outputs found
Rapid ultrasensitive chemometrics-fluorescence methodology to quantifyfluoroquinolones antibiotics residues in surface water
A sensitive method for the determination of fluoroquinolones in surface waters at trace concentration level is presented. The proposed two-step methodology consists in a solid-phase extraction using C-18 membranes followed measurement of the emission molecular fluorescence spectra over extracted membrane without elution of the analytes. Membrane background signal was removed by the used of chemometrics calculations, in addition chemometrics was as well used for the direct and simultaneous determination of the studied compounds. The method was optimized for the analysis of three fluoroquinolones: enoxacin (ENO), norfloxacin (NOR) and ofloxacin (OFLO). The fluorescence of these compounds increase drastically when they are into the membrane, thus with this method low concentrations are possible to be determined, as the concentration in which these compounds appear in surface water. Limits of detection at the ng • L⁻¹ level were estimated for ENO, NOR and OFLO
Simultano UV-spektrofotometrijsko određivanje ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u kapsulama primjenom kemometrijskih metoda
In the present work, three different spectrophotometric methods for simultaneous estimation of ramipril, aspirin and atorvastatin calcium in raw materials and in formulations are described. Overlapped data was quantitatively resolved by using chemometric methods, viz. inverse least squares (ILS), principal component regression (PCR) and partial least squares (PLS). Calibrations were constructed using the absorption data matrix corresponding to the concentration data matrix. The linearity range was found to be 1-5, 10-50 and 2-10 µg mL–1 for ramipril, aspirin and atorvastatin calcium, respectively. The absorbance matrix was obtained by measuring the zero-order absorbance in the wavelength range between 210 and 320 nm. A training set design of the concentration data corresponding to the ramipril, aspirin and atorvastatin calcium mixtures was organized statistically to maximize the information content from the spectra and to minimize the error of multivariate calibrations. By applying the respective algorithms for PLS 1, PCR and ILS to the measured spectra of the calibration set, a suitable model was obtained. This model was selected on the basis of RMSECV and RMSEP values. The same was applied to the prediction set and capsule formulation. Mean recoveries of the commercial formulation set together with other figures of merit (calibration sensitivity, selectivity, limit of detection, limit of quantification and analytical sensitivity) were estimated. Validity of the proposed approaches was successfully assessed for analyses of drugs in the various prepared physical mixtures and formulations.U radu su opisane tri različite spektrofotometrijske metode za određivanje ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u sirovinama i formulacijama. Preklapanje podataka kvantitativno je riješeno pomoću kemometrijskih metoda, tj. metodama inverznih najmanjih kvadrata (ILS), regresije glavnog sastojka (PCR) i djelomičnih najmanjih kvadrata (PLS). Kalibracije su postavljene pomoću matrice podataka za apsorpciju koja odgovara matrici pripadajućih koncentracija. Područje linearnosti za ramipril iznosilo je 1–5, za acetilsalicilnu kiselinu 10–50, a za atorvastatin kalcij 2–10 µg mL–1. Matrica s apsorbancijama dobivena je mjerenjem apsorbancije nultog reda na valnim duljinama između 210 i 320 nm. Set podataka za koncentracije ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u smjesi statistički je tako organiziran da osigura maksimalnu količinu informacije u spektrima i minimalizira grešku multivarijantnih kalibracija. Primjenom odgovarajućih algoritama za PLS, PCR i ILS na snimljene spektre kalibracijskog seta dobiven je dobar model, koji je odabran na temelju RMSECV i RMSEP vrijednosti. Isti model je primijenjen i na set s predviđenim vrijednostima i na kapsule sa smjesom ove tri ljekovite tvari. Određena je srednja vrijednost povrata za komercijalnu formulaciju te ostale analitičke izvedbene značajke (kalibracijska osjetljivost, selektivnost, granica dokazivanja, granica određivanja i analitička osjetljivost). Potvrđena je primjenjljivost predloženih metoda u analizama lijekova u fizičkim smjesama i u gotovim ljekovitim oblicima
A simple and sensitive method for determination of Norfloxacin in pharmaceutical preparations
In this approach, a new voltammetric method for determination of norfloxacin was proposed with high sensitivity and wider detection linear range. The used voltammetric sensor was fabricated simply by coating a layer of graphene oxide (GO) and Nafion composited film on glassy carbon electrode. The advantage of proposed method was sensitive electrochemical response for norfloxacin, which was attributed to the excellent electrical conductivity of GO and the accumulating function of Nafion under optimum experimental conditions, the present method revealed a good linear response for determination of norfloxacin in the range of 1×10-8mol/L-7×10-6 mol/L with a detection limit of 5×10-9 mol/L. The proposed method was successfully applied in the determination of norfloxacin in capsules with satisfactory results.</p
A Fluorescent Probe for Diacetyl Detection
A water-soluble fluorescent probe, rhodamine B hydrazide (RBH), was prepared and its properties for recognition of diacetyl were studied. The method employs the reaction of diacetyl with RBH, a colorless and non-fluorescent rhodamine B spiro form derivative to give a pink-colored fluorescent substance. In weakly acidic media, RBH reacts more selectively with diacetyl than with other carbonyls, causing a large increase in fluorescence intensity and thereby providing an easy assay for the determination of diacetyl
Elective Cancer Surgery in COVID-19-Free Surgical Pathways During the SARS-CoV-2 Pandemic: An International, Multicenter, Comparative Cohort Study.
PURPOSE: As cancer surgery restarts after the first COVID-19 wave, health care providers urgently require data to determine where elective surgery is best performed. This study aimed to determine whether COVID-19-free surgical pathways were associated with lower postoperative pulmonary complication rates compared with hospitals with no defined pathway. PATIENTS AND METHODS: This international, multicenter cohort study included patients who underwent elective surgery for 10 solid cancer types without preoperative suspicion of SARS-CoV-2. Participating hospitals included patients from local emergence of SARS-CoV-2 until April 19, 2020. At the time of surgery, hospitals were defined as having a COVID-19-free surgical pathway (complete segregation of the operating theater, critical care, and inpatient ward areas) or no defined pathway (incomplete or no segregation, areas shared with patients with COVID-19). The primary outcome was 30-day postoperative pulmonary complications (pneumonia, acute respiratory distress syndrome, unexpected ventilation). RESULTS: Of 9,171 patients from 447 hospitals in 55 countries, 2,481 were operated on in COVID-19-free surgical pathways. Patients who underwent surgery within COVID-19-free surgical pathways were younger with fewer comorbidities than those in hospitals with no defined pathway but with similar proportions of major surgery. After adjustment, pulmonary complication rates were lower with COVID-19-free surgical pathways (2.2% v 4.9%; adjusted odds ratio [aOR], 0.62; 95% CI, 0.44 to 0.86). This was consistent in sensitivity analyses for low-risk patients (American Society of Anesthesiologists grade 1/2), propensity score-matched models, and patients with negative SARS-CoV-2 preoperative tests. The postoperative SARS-CoV-2 infection rate was also lower in COVID-19-free surgical pathways (2.1% v 3.6%; aOR, 0.53; 95% CI, 0.36 to 0.76). CONCLUSION: Within available resources, dedicated COVID-19-free surgical pathways should be established to provide safe elective cancer surgery during current and before future SARS-CoV-2 outbreaks
Elective cancer surgery in COVID-19-free surgical pathways during the SARS-CoV-2 pandemic: An international, multicenter, comparative cohort study
PURPOSE As cancer surgery restarts after the first COVID-19 wave, health care providers urgently require data to determine where elective surgery is best performed. This study aimed to determine whether COVID-19–free surgical pathways were associated with lower postoperative pulmonary complication rates compared with hospitals with no defined pathway. PATIENTS AND METHODS This international, multicenter cohort study included patients who underwent elective surgery for 10 solid cancer types without preoperative suspicion of SARS-CoV-2. Participating hospitals included patients from local emergence of SARS-CoV-2 until April 19, 2020. At the time of surgery, hospitals were defined as having a COVID-19–free surgical pathway (complete segregation of the operating theater, critical care, and inpatient ward areas) or no defined pathway (incomplete or no segregation, areas shared with patients with COVID-19). The primary outcome was 30-day postoperative pulmonary complications (pneumonia, acute respiratory distress syndrome, unexpected ventilation). RESULTS Of 9,171 patients from 447 hospitals in 55 countries, 2,481 were operated on in COVID-19–free surgical pathways. Patients who underwent surgery within COVID-19–free surgical pathways were younger with fewer comorbidities than those in hospitals with no defined pathway but with similar proportions of major surgery. After adjustment, pulmonary complication rates were lower with COVID-19–free surgical pathways (2.2% v 4.9%; adjusted odds ratio [aOR], 0.62; 95% CI, 0.44 to 0.86). This was consistent in sensitivity analyses for low-risk patients (American Society of Anesthesiologists grade 1/2), propensity score–matched models, and patients with negative SARS-CoV-2 preoperative tests. The postoperative SARS-CoV-2 infection rate was also lower in COVID-19–free surgical pathways (2.1% v 3.6%; aOR, 0.53; 95% CI, 0.36 to 0.76). CONCLUSION Within available resources, dedicated COVID-19–free surgical pathways should be established to provide safe elective cancer surgery during current and before future SARS-CoV-2 outbreaks
Rapid Ultrasensitive Chemometrics-Fluorescence Methodology To Quantify Fluoroquinolones Antibiotics Residues In Surface Water
A sensitive method for the determination of fluoroquinolones in surface waters at trace concentration level is presented. The proposed two-step methodology consists in a solid-phase extraction using C-18 membranes followed measurement of the emission molecular fluorescence spectra over extracted membrane without elution of the analytes. Membrane background signal was removed by the used of chemometrics calculations, in addition chemometrics was as well used for the direct and simultaneous determination of the studied compounds. The method was optimized for the analysis of three fluoroquinolones: enoxacin (ENO), norfloxacin (NOR) and ofloxacin (OFLO). The fluorescence of these compounds increase drastically when they are in the membrane, thus with this method low concentrations are possible to be determined, as the concentration in which these compounds appear in surface water. Limits of detection at the ng•L–1 level were estimated for ENO, NOR and OFLO
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