Search results for " Limit"
showing 10 items of 1716 documents
FI-chemiluminometric study of thiazides by on-line photochemical reaction
2004
The present manuscript deals with a simple and sensitive flow-injection method for the chemiluminescent determination of thiazides. The method is based on the on-line photodegradation and chemiluminescent determination of the resulting photo-fragments. The on-line photodegradation is performed in basic medium by using a photoreactor consisting of a 550 cm long x 0.8 mm ID piece of PTFE tubing helically coiled around an 8 W low-pressure mercury lamp. The determination of the photo-irradiated thiazides is performed by a chemiluminescent oxidative reaction with Ce(IV) in sulphuric acid medium. A heterogeneous group of thiazides (indapamide, metolazone, hydroflumethiazide, chlorthalidone and be…
On-line gradient liquid chromatography–Fourier transform infrared spectrometry determination of sugars in beverages using chemometric background corr…
2008
Abstract An on-line gradient reversed phase liquid chromatography–Fourier transform infrared spectrometry (LC–FTIR) method was developed for the determination of fructose, glucose, sucrose and maltose in beverages. Improved chromatographic resolution was obtained using a linear gradient from 75 to 55% (v/v) acetonitrile in water in 15 min. Changes in the background spectra were corrected employing “univariate background correction based on the use of a reference spectra matrix” (UBC-RSM) and using the ratio of absorbance (AR) at 2256 and 2253 cm −1 for the identification of the eluent spectra within the RSM. The method provided limits of detection in the order of 0.75 mg ml −1 . The precisi…
An in-tube SPME device for the selective determination of chlorophyll a in aquatic systems.
2010
We report a new device for the estimation of the content of chlorophyll a pigment in water samples as an indicator of water quality. The extraction of the pigment from water was also optimized. 10 mL of water was filtered through a nylon filter (45m pore size and 13 mm of diameter), after the chlorophylls were dissolved by immersing the filter in 1 mL of a low non-hazardous solvent as ethanol. An in-valve in-tube SPME device coupled to capillary liquid chromatography with diode array detection was designed. A capillary column of 70 cm in length (0.32 mm i.d. coated with 5% diphenyl–95% polydimethylsiloxane, 3m coating thickness) was used as the loop of the injection valve for preconcentrati…
Gas chromatographic analysis of resveratrol in plasma, lipoproteins and cells after in vitro incubations
1998
Resveratrol is a trihydroxystilbene present in certain red wines. It may play a role in the inhibition of lipoprotein oxidation and platelet activity. We have developed the first method to measure resveratrol in animal and human samples and to study its incorporation in vitro. After adding epicoprostanol as an internal standard, samples are subjected to lipid extraction in the presence of antioxidant and under dim light to minimize both denaturation and isomerization of the trans-resveratrol to the cis-form. Extracts were purified by cold acetone precipitation and the resveratrol-containing acetone phase was evaporated under nitrogen. The resveratrol was analyzed as a trimethylsilyl derivat…
Determination of organochlorine pesticide residues in honey from the central zone of Portugal and the Valencian community of Spain
2004
In this study nine organochlorine pesticide residues ([alpha]-, [beta]-, and [gamma]-hexachlorocyclohexane (HCH), hexachlorobenzene (HCB), aldrin, p,p'-DDE, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in forty nine samples of honey collected from markets of Portugal and Spain during 2001 and 2002, respectively, were evaluated. For this evaluation, three analytical procedures were studied. The analytical procedure, based on LLE extraction with ethyl acetate followed by gas chromatography-electron-capture detection (GC-ECD) for quantification, and mass spectrometry (GC-MS) for confirmation, has been selected. Recoveries of spiked samples ranged from 68%, for [beta]-HCH, and 126% for p,p'-DDT, for forti…
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…
A new selective fluorogenic probe for trivalent cations.
2012
[EN] A new selective chromo-fluorogenic probe for Fe 3+, Cr 3+ and Al 3+ is reported. Detection limits are in the ¿M range and the fluorogenic sensing ability could be observed by the naked eye when illuminated with UV-light. No response is observed with divalent cations. © 2012 The Royal Society of Chemistry.
Extraction of polycyclic aromatic hydrocarbons from cookies: a comparative study of ultrasound and microwave-assisted procedures.
2008
The chromatographic determination of 15 polycyclic aromatic hydrocarbons (PAHs) in cookies has been improved in order to obtain a fast method with a low limit of detection through the combination of microwave-assisted extraction (MAE), oil saponification and solid-phase extraction clean-up before the injection of purified extracts in a C18 201TP52 (5 microm, 250 x 2.1 mm) column. Using acetonitrile-water as mobile phase, with a 50% to 95% w/w acetonitrile gradient for a fixed flow of 0.250 ml min(-1), 15 PAHs were separated in 45 min. The column temperature was maintained at 15 degrees C; and fluorimetric detection was made at a fixed excitation wavelength of 264 nm and emission measurement…
Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometric analysis of benzoylurea insecticides in citrus fruits.
2000
A liquid chromatography (LC) method for the quantitative determination of three benzoylurea insecticide residues (diflubenzuron, flufenoxuron and hexaflumuron) in citrus fruits is described. Residues were successfully separated on a C18 column by methanol/water gradient elution. Detection was by negative-ion, selected-ion monitoring atmospheric pressure chemical ionization-mass spectrometry (APCI-MS); the main ions were [M - H]-, and the secondary fragment ions were [M - H - HF]-. Useful confirmatory information can thus be obtained at low extraction voltages from losses of HF. Detection limits for standard solutions were 10 fg injected and good linearity and reproducibility were obtained. …
Pesticide residues in oranges from Valencia (Spain)
2001
One hundred and fifty citrus samples from an agricultural co-operative of the Valencian Community (Spain) were analysed for pre- and post-harvest pesticide residues using high performance liquid chromatography and gas chromatography. Among the residues from post-harvest treatments, imazalil was detected in 112 (74.7%) samples at a mean level of 1.2 mg/kg, thiabendazole in 21 (14.0%) samples at a mean level of 0.47 mg/kg and carbendazim in 5 (3.3%) samples at a mean level of 1.05 mg/kg. Among the residues from pre-harvest treatment, dicofol was detected in 28 (18.7%) samples at a mean level of .28 mg/kg chlorpyriphos in 19 (12.7% samples at a mean level of 0.16 mg/kg and endosulfan in 11 (7.…