Search results for "analytical"
showing 10 items of 9586 documents
Assisted baseline subtraction in complex chromatograms using the BEADS algorithm.
2017
The data processing step of complex signals in high-performance liquid chromatography may constitute a bottleneck to obtain significant information from chromatograms. Data pre-processing should be preferably done with little (or no) user supervision, for a maximal benefit and highest speed. In this work, a tool for the configuration of a state-of-the-art baseline subtraction algorithm, called BEADS (Baseline Estimation And Denoising using Sparsity) is developed and verified. A quality criterion based on the measurement of the autocorrelation level was designed to select the most suitable working parameters to obtain the best baseline. The use of a log transformation of the signal attenuate…
Optimised procedures for the reversed-phase liquid chromatographic analysis of formulations containing tricyclic antidepressants.
2003
The chromatographic behaviour (retention, selectivity, peak shape and resolution) of seven tricyclic antidepressants (TCAs), amitryptiline, clomipramine, doxepin, imipramine, maprotiline, nortryptiline and trimipramine, was examined. Conventional unendcapped Cs and C18 columns and an endcapped XTerra MS C18 column recommended for the analysis of basic compounds were used together with acetonitrile-water and micellar sodium dodecylsulfate (SDS)-pentanol mobile phases. The two best combinations were XTerra C18/acetonitrile, which yielded the largest efficiencies and resolution, and C8/SDS-pentanol, which eliminated the peak tails that were still observed with the XTerra C18 column. Both the s…
Reversed phase liquid chromatography for the enantioseparation of local anaesthetics in polysaccharide-based stationary phases. Application to biodeg…
2020
[EN] A comprehensive study on the chiral separation of bupivacaine, mepivacaine, prilocaine and propanocaine with eight commercial polysaccharide-based chiral stationary phases (CSPs) in reversed phase conditions compatible with MS detection is performed. Methanol and acetonitrile are used as organic modifiers. Retention and resolution values obtained for each compound in the different CSPs and mobile phases are compared. The polysaccharide-based CSPs tested present different enantioselectivity towards the analytes. From the results, the experimental conditions for determining the enantiomers of bupivacaine, mepivacaine, prilocaine and propanocaine in saline aqueous samples using MS detecti…
A capillary liquid chromatography method for benzalkonium chloride determination as a component or contaminant in mixtures of biocides
2015
A method for quantifying benzalkonium chloride (BAK), an alkyl dimethyl benzyl ammonium compound, in several biocides formulations is proposed. A tertiary amine like N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine (TA) and a straight-chain alkyl ammonium compound like trimethyl-tetradecyl ammonium chloride (TMTDAC), have been employed as trade surfactants besides BAK. Two capillary analytical columns with different polarities are tested: inertsil CN-3 capillary column (150mm×0.5mm i.d., 3μm particle diameter) and a non endcapped Zorbax C18 capillary column (35mm×0.5mm i.d., 5μm particle diameter). This latter column provided the best separation of the BAK homologues in less than 12min using …
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…
Agrobacterium tumefaciens-mediated genetic transformation of the cardenolide-producing plant Digitalis minor L.
2003
A repeatable transformation system has been established for Digitalis minor using Agrobacterium tumefaciens. Leaf explants from 30-day-old seedlings were inoculated with either EHA105 (carrying the nptII and gusA genes) or AGL1 (with the bar and gusA genes) strains. Among the tested factors influencing T-DNA transfer to plants, the EHA105 strain and the addition of acetosyringone to the co-culture medium increased transformation. The highest transformation efficiency (8.4%) was obtained when freshly isolated explants, soaked in a bacterial suspension with an OD 550 of 0.9, were subcultured on selection medium after a 4-day co-culture with the bacteria. Evidence of stable transgene integrati…
Ferro-pedrizite, NaLi2(Fe2+ 2Al2Li)Si8O22(OH)2, a new amphibole-supergroup mineral from the Sutlug pegmatite, Tyva Republic, Russia
2015
Ferro-pedrizite, a new amphibole-supergroup mineral was discovered in the Sutlug pegmatite occurrence situated in the Targi River Basin, Tyva Republic, Eastern Sibera, Russia. The associated minerals are quartz, albite, microcline, spodumene, cassiterite, beryl, columbite-(Mn), fergusonite-β-(Y), fluorapatite, schorl, trilithionite and fluorite. Ferro-pedrizite forms dark grey-blue to violet-blue acicular and long prismatic crystals up to 2 × 5 × 50 mm and their aggregates. D meas = 3.16(1) g/cm3 (by hydrostatic weighing), 3.13(1) g/cm3 (by flotation in heavy liquids); D calc = 3.135 g/cm3. Ferro-pedrizite is optically biaxial (−), α = 1.614(3), β = 1.638(3), γ = 1.653(3), 2 V meas = 75(5)°…
Crystal fabrics and element impurities (Sr/Ca, Mg/Ca, and Ba/Ca) in shells of Arctica islandica—Implications for paleoclimate reconstructions
2013
Sr/Ca, Mg/Ca and Ba/Ca values are heterogeneously distributed in shells of Arctica islandica. These patterns are largely associated with crystal fabrics (size, habit and orientation of crystals) or the processes controlling them. The outer sublayer of the outer shell layer (oOSL; homogenous and irregular simple prismatic crystal fabrics,) contained element/Ca values up to 62% higher than the inner sublayer (iOSL; crossed-acicular, crossed-lamellar, fine crossed-lamellar and irregular simple prismatic crystal fabrics). A gradual decrease in Sr/Ca and Mg/Ca values was observed from the outer portions of the oOSL toward the oOSL/iOSL transition zone. This chemical shift was accompanied by a gr…
Some observations on the determination of total heavy metals in sewage sludge by atomic absorption spectrophotometry after a pressurized acid digesti…
1990
Abstract An economical and simple method for the flame atomic absorption spectrometric determination of Cd, Pb, Ni, Cu, Fe, and Zn in sewage sludges is described. Samples are treated with concentrated HNO 3 in a thermal oven using Pyrex glass tubes hermetically sealed with Bakelite screw caps. The effect of the digestion parameters, such as digestion time, acid volume, sample mass, and temperature, were studied. The precision and accuracy of this procedure were evaluated by the analysis of two BCR (Community Bureau of Reference, European Communities) certified sewage sludge samples (CRM 146 and 144).
Flame atomic absorption analysis of gold in jewelry samples
1990
A new procedure is proposed for the determination of gold by flame atomic absorption in jewelry samples. The method is based on the acid digestion of 10 mg of sample in a microwave oven and on the on-line dilution, using a three-way valve. The dynamic range of the technique is extended to 100 mg/l gold solutions and using a weighted bracketing method for the treatment of the results, accuracy errors lower than 2% can be found in the analysis of real samples as compared with those obtained by fire assay. The method is very fast and implies only little damage to the jewelry samples.