Search results for " Limit"
showing 10 items of 1716 documents
Spectrophotometric determination of ethiofencarb in waters by reaction with p-aminophenol
1993
An automatized procedure has been developed for the spectrophotometric determination of ethiofencarb in water by reaction with p-aminophenol after alkaline hydrolysis to obtain the corresponding phenol sulphone. The hydrolyzed samples are continuously introduced into different manifolds at the same time as 300 mg/l p-aminophenol, 0.004 mol/l KIO4 and 0.04 mol/l NaOH solutions. The absorbance is measured at 638 nm after a reaction time of 6 min in stop flow. This absorbance band corresponds to the indo dye obtained from the reaction between the phenol sulphone of ethiofencarb and the quinoneimine form of the p-aminophenol and it permits a matrix-free spectrophotometric determination of ethio…
Development of microextraction techniques in combination with GC-MS/MS for the determination of mycotoxins and metabolites in human urine.
2017
Simple and highly efficient sample preparation procedures, namely, dispersive liquid–liquid microextraction and salting-out liquid–liquid extraction for the analysis of ten Fusarium mycotoxins and metabolites in human urine were compared. Various parameters affecting extraction efficiency were carefully evaluated. Under optimal extraction conditions, salting-out liquid–liquid extraction showed a better accuracy (84–96%) and precision (<14%) than dispersive liquid–liquid microextraction. Hence, a multibiomarker method based on salting-out liquid–liquid extraction followed by gas chromatography with tandem mass spectrometry was proposed. Satisfactory results in terms of validation were achiev…
Isocratic high-performance liquid chromatographic determination of tryptophan in infant formulas.
1996
The application to infant formulas of a method for tryptophan determination by isocratic HPLC with UV detection at 254 nm, after derivatization with phenyl isothiocyanate, was studied. Protein was hydrolysed by barium hydroxide at 120 degrees C for 8 h, followed by derivatization with phenyl isothiocyanate, HPLC and UV detection at 254 nm. The optimum chromatographic conditions (pH, ionic strength of elution solvent and eluent ratio) were established. The analytical parameters (linearity, precision, accuracy of derivatization and limits of detection and quantification) were determined. The values obtained demonstrated that the method is useful for determining the tryptophan content of infan…
Determination of free formaldehyde in cosmetics containing formaldehyde-releasing preservatives by reversed-phase dispersive liquid-liquid microextra…
2017
Abstract An analytical method for the determination of traces of formaldehyde in cosmetic products containing formaldehyde-releasing preservatives has been developed. The method is based on reversed-phase dispersive liquid–liquid microextraction (RP-DLLME), that allows the extraction of highly polar compounds, followed by liquid chromatography–ultraviolet/visible (LC–UV/vis) determination with post-column derivatization. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the selected conditions, a mixture of 500 μL of acetonitrile (disperser solvent) and 50 μL of water (extraction solvent) was rapidly injected into 5 mL of toluene sampl…
Sample Preparation Improvement in Polycyclic Aromatic Hydrocarbons Determination in Olive Oils by Gel Permeation Chromatography and Liquid Chromatogr…
2005
Abstract The determination of 15 polycyclic aromatic hydrocarbons (PAHs) in olive oil samples has been improved in order to obtain a fast methodology with a low limit of detection through the combination of liquid–liquid extraction with acetonitrile and preparative gel permeation chromatography (GPC) prior to the injection of purified extracts into a C18 column. Acetonitrile–water was used as the mobile phase with a gradient from 50 to 95%, w/w, acetonitrile in 30 min. The oven temperature was maintained at 15°C, and fluorometric detection was made at a fixed excitation wavelength of 264 nm and variable, optimal emission wavelength for each analyte ranging from 352 nm for 11-H-benzo(b)fluor…
Psychological State after an Acute Coronary Syndrome: Impact of Physical Limitations
2021
The aim of this study was to investigate how physical limitations after ACS influence patients’ quality of life and health perception. This was a longitudinal clinical study. We recruited 146 patients diagnosed with ACS. The patients performed a stress test (Bruce’s protocol) for the evaluation of physical limitations and were classified according to the test result: without physical limitations (more than 10 METS), with some physical limitations (7 to 9 METS), and with high physical limitations (less than 6 METS). Significant differences were found between the three groups immediately after the diagnosis of ACS and after a period of three months, regarding health perception, anxiety, depre…
Dialettica al limite
2018
L'appello di Th W. Adorno a forme non antagonistiche di coesistenza del diverso, intese come modelli di razionalità in cui il non identico non cada sotto il bando della logica identitaria, costituisce un nodo fortemente problematico che investe in modo radicale il senso, nonché la sopravvivenza stessa, della dialettica, almeno così come essa viene concepita dal filosofo francofortese. Raccogliere i suggerimenti di Adorno in direzione del pensare in costellazioni, o anche in direzione di una dialettica che deve riappropriarsi della sua originaria radice linguistica per farsi esperienza comunicativa del differenziato, significa infatti dover seguire una strada che, però, se fosse percorsa fin…
Micellar Liquid Chromatography: A Worthy Technique for the Determination of β-Antagonists in Urine Samples
1998
Several beta-antagonists (acebutolol, atenolol, celiprolol, labetalol, metoprolol, nadolol, propranolol) were determined in urine samples with fluorometric detection after direct injection, in less than 15 min, with a micellar mobile phase of 0.1 M sodium dodecyl sulfate (SDS), 15% propanol, and 1% triethylamine at pH 3. The limits of detection (38 criterion) were usually between 3 and 30 ng/mL. The addition of propanol and triethylamine and the reduction of the pH of the mobile phase improved the efficiency of the chromatographic peaks that was rather low in pure micellar eluents. The selection of the composition of the mobile phase was easily performed through the use of an interpretive p…
Determination of 21 perfluoroalkyl substances and organophosphorus compounds in breast milk by liquid chromatography coupled to orbitrap high-resolut…
2018
Abstract The human exposure to perfluoroalkyl (PFASs) and organophosphorus (OPs) compounds is a cause of concern and its determination in biological matrices, including human milk, is an emergent approach for evaluate their exposure. A comprehensive strategy for the quantitative determination of 21 PFASs and OPs compounds in breast milk was developed. The proposed method includes an extraction and clean-up procedure based on the QuEChERs methodology followed by an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) determination. The full-scan mass data were acquired with a resolution of 50000 FWHM and a mass accuracy better than 5 ppm. Met…
On-Capillary Surface-Enhanced Raman Spectroscopy: Determination of Glutathione in Whole Blood Microsamples.
2018
Oxidative stress monitoring in the neonatal period supports early outcome prediction and treatment. Glutathione (GSH) is the most abundant antioxidant in most cells and tissues, including whole blood, and its usefulness as a biomarker has been known for decades. To date, the available methods for GSH determination require laborious sample processing and the use of sophisticated laboratory equipment. To the best of our knowledge, no tools suitable for point-of-care (POC) sensing have been reported. Surface-enhanced Raman spectroscopy (SERS), performed in a microvolume capillary measurement cell, is proposed in this study as a robust approach for the quantification of GSH in human whole blood…