Search results for "ESOL"
showing 10 items of 2444 documents
Determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in goat milk and tissues by glass capillary gas chromatography and medium resolution mass fragme…
1981
Abstract An analytical method has been developed for the study of the elimination of 2,3,7,8-tetrachlodoribenzo-p-dioxin (TCDD) by lactation and its determination in various tissues of goat. The method is based on the alkaline hydrolysis of milk, liver, fat, muscle, blood, faeces and urine samples, extraction with n-hexane, treatment with sulphuric acid-saturated silica gel, chromatographic clean-up on silica gel and alumina micro-columns, and glass capillary gas chromatography—medium resolution mass fragmenography (resolution 2000). 1,2,3,4-Tetrachlorodibenzo-p-dioxin is used as the internal standard, the concentration of TCDD being determined from the calibration curve calculated from the…
Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.
2009
Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise f…
Finding the best separation in situations of extremely low chromatographic resolution.
2010
Abstract Samples with a large number of compounds or similarities in their structure and polarity may yield insufficient chromatographic resolution. In such cases, however, finding conditions where the largest number of compounds appears sufficiently resolved can be still worthwhile. A strategy is here reported that optimises the resolution level of chromatograms in cases where conventional global criteria, such as the worst resolved peak pair or the product of elementary resolutions, are not able to detect any separation, even when most peaks are baseline resolved. The strategy applies a function based on the number of “well resolved” peaks, which are those that exceed a given threshold of…
1-Hexyl-3-methyl imidazolium tetrafluoroborate: an efficient column enhancer for the separation of basic drugs by reversed-phase liquid chromatograph…
2012
Abstract Ionic liquids are dual modifiers composed by a large anion and a large cation, which interact with both the hydrophobic alkyl-bonded phase and the anionic residual silanols in C18 columns. The deactivation of the silanol groups has important implications on the chromatographic analysis of basic drugs, being the improvement of peak profiles and shorter retention times the most noticeable features. However, other characteristics as selectivity or resolution are not usually considered, or are only examined for selected chromatographic conditions. In this work, the effect of the addition of the ionic liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate to acetonitrile–water mixtures i…
A complementary mobile phase approach based on the peak count concept oriented to the full resolution of complex mixtures
2011
Situations of minimal resolution are often found in liquid chromatography, when samples that contain a large number of compounds, or highly similar in terms of structure and/or polarity, are analysed. This makes full resolution with a single separation condition (e.g., mobile phase, gradient or column) unfeasible. In this work, the optimisation of the resolution of such samples in reversed-phase liquid chromatography is approached using two or more isocratic mobile phases with a complementary resolution behaviour (complementary mobile phases, CMPs). Each mobile phase is dedicated to the separation of a group of compounds. The CMPs are selected in such a way that, when the separation is cons…
A rapid and sensitive method for the control of selected regulated and emerging mycotoxins in beer
2018
A fast method using automated online solid-phase extraction (SPE) coupled to liquid-chromatography/high resolution mass spectrometric (LC-HRMS) detection for the determination of 12 mycotoxins in beer was developed and fully validated according to the performance criteria set in the European Union (EU) guidelines. Mycotoxin detection was achieved by full-scan HRMS with electrospray ionisation in positive ion mode within 13 min. No significant matrix interferences were observed. The lowest limits of detection (LODs) were achieved for emerging mycotoxins (beauvericin and enniatins) and ochratoxin A at levels between 0.01 and 0.02 μg/l, while the overall LODs were in the range of 0.01-0.30 μg…
Spectrophotometric determination of chlorhexidine with bromocresol green by flow-injection and manual methods
1986
Abstract A spectrophotometric study of the chlorhexidine/bromocresol green/Triton X-100 system is reported; at pH 5.3, both 2:1 and 1:1 bromocresol green/chlorhexidine complexes are formed. In the manual spectrophotometric method, Beer's law is obeyed for chlorhexidine concentrations of 2.9–32.2 μg ml −1 (r.s.d. 0.4–1.3%); the molar absorptivity is 12 500 l mol −1 cm −1 . In the flow-injection method, the calibration graph is linear for the chlorhexidine range 23.0–83.9 μg ml −1 (r.s.d. 0.8%); the injection is ca. 60 h −1 . Benzocaine, acetylsalicylic acid, ascorbic acid and sucrose are tolerated at 10 −2 −10 −3 M levels. Hibitane 5% was analyzed successfully.
Thin-layer chromatography of 2-methyl-4-chlorophenoxyacetic acid and its soil metabolites
1980
Abstract The thin-layer chromatography of 2-methyl-4-chlorophenoxyacetic acid, 4-chloro- o -cresol and 3-methyl-5-chlorocatechol and their pentafluorobenzyl derivatives has been studied on silica gel as adsorbent with 19 solvent systems. The best separation of the individual components occurred with toluene-benzene-acetic acid (2:2:1). Chloroform-diethyl ether-toluene (1:1:1) was suitable for the group separation of the pentafluorobenzyl derivatives.
Extractive Spectrophotometric Determination of Ondansetron by Ion-Pair Formation with Bromocresol Green
1996
Abstract An empirical spectrophotometric procedure for the determination of the antiemetic ondansetron is carried out. The method is based on the formation of a 1:1 ion pair with bromocresol green in the pH range over 3.2 – 4.4, extraction into chloroform layer and spectrophotometric measurement at 420.8 nm. The calibration graph is linear over the range 0.1 – 20 μg ml−1 ondansetron, with a relative standard deviation of 2.7%; the influence of foreign substances is also studied. The method is applied to ondansetron determination in human urine.
Peak deconvolution in one-dimensional chromatography using a two-way data approach.
2002
A deconvolution methodology for overlapped chromatographic signals is proposed. Several single-wavelength chromatograms of binary mixtures, obtained in different runs at diverse concentration ratios of the individual components, were simultaneously processed (multi-batch approach), after being arranged as two-way data. The chromatograms were modelled as linear combinations of forced peak profiles according to a polynomially modified Gaussian equation. The fitting was performed with a previously reported hybrid genetic algorithm with local search, leaving all model parameters free. The approach yielded more accurate solutions than those found when each experimental chromatogram was fitted in…