Search results for "DETECT"
showing 10 items of 5902 documents
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…
RP-HPLC-DAD determination of the differences in the polyphenol content of Fucus vesiculosus extracts with similar antioxidant activity.
2021
Abstract Significant quantities of bioactive compounds have been found in the chemical composition of seaweeds. This source of natural antioxidants such as polyphenols appears to attenuate lipid peroxidation caused by oxidative stress, preventing the harmful effects of a number of injuries including ischemia–reperfusion (I/R). Conventional extraction (CE) has been used for years as a traditional method for obtaining bioactive components from seaweeds. However, recent studies highlight ultrasonic-assisted extraction (UAE) as an alternative and more eco-friendly technique. Therefore, the two methods were optimised and compared to obtain a Fucus vesiculosus extract (FVE) with high antioxidant …
Comparison of photodiode array, evaporative light scattering, and single-quadrupole mass spectrometric detection methods for the UPLC analysis of pyr…
2017
ABSTRACTIt is important to analyze pyrolysis liquids to evaluate the yield of valuable products as well as unfavorable by-products. This work focuses on choosing detectors for reversed-phase ultra high-performance liquid chromatography analysis of pyrolysis liquids. The linearity, sensitivity, precision, and recovery of photodiode array (PDA) detector, single-quadrupole mass spectrometer (MS), and evaporative light scattering (ELS) detector were compared for the quantitative determination of several typical compounds found in pyrolysis liquids. PDA and MS detectors were found to be suitable for the quantification of furans and phenol derivatives (furfural, vanillin, syringol), but sugars an…
Gas chromatographic and mass spectrometric analysis of chlorinated catechols occurring in pulp bleach liquors
1982
Chlorination step (C-step), spent bleach liquor from a kraft pulp mill and the product from the chlorination of guaiacol in aqueous solution have been investigated for their content of chlorinated catechols. After separation the samples were derivatized with diazoethane and analysed by glass capillary gas chromatography with an electron capture detector. The external standard mixture of all ethylated chlorocatechols was used in the measurements. The structures of the compounds identified were confirmed by gas chromatography/mass spectrometry. Eight chlorinated catechols were identified from a sample prepared by chlorination of guaiacol with Cl2 in aqueous solution. However, only four of the…
High-resolution pyrolysis–gas chromatography with a movable reaction zone
1997
Abstract A new device was constructed for pyrolysis–gas chromatography and it was laboratory tested. The device enables the thermal degradation of polymers inside a capillary pre-column and transfer of the reaction zone into a column oven. The pyrolysis procedure described protects the thermally sensitive compounds prior to pyrolysis, prevents the process of irreversible condensation of high-boiling pyrolysis products during the chromatographic process and eliminates extracolumn effects on the peak broadening.
Development of a new multi-analyte assay for the simultaneous detection of opioids in serum and other body fluids using liquid chromatography-tandem …
2015
Abstract A liquid chromatography–tandem mass spectrometry method using electrospray ionization in positive ionization mode was developed for the simultaneous detection of multiple opioid-type drugs in plasma. The presented assay allows the quantitative determination of alfentanil, buprenorphine, codeine, desomorphine, dextromethorphan, dextrorphan, dihydrocodeine, dihydromorphine, ethylmorphine, fentanyl, hydrocodone, hydromorphone, methadone, morphine, naloxone, naltrexone, oxycodone, oxymorphone, pentazocine, pethidine, pholcodine, piritramide, remifentanil, sufentanil, and tramadol as well as the metabolites 6-monoacetylmorphine, bisnortilidine, morphine-3-glucuronide, morphine-6-glucuro…
Packing technology, column bed structure and chromatographic performance of 1-2-μm non-porous silicas in high-performance liquid chromatography
1989
This work is aimed at further elucidating the aggregation behaviour of micron- and submicron-size non-porous silicas and the column performance of 1–2-μm C18 silicas in reversed-phase high-performance liquid chromatography of low-molecular weight compounds. It is demonstrated that highly ordered, dense, porous aggregates of such silica beads were obtained by gravity settling and centrifugation. The slurry techniques applied at constant flow-rate and a pressure up to 50 MPa provided less-ordered aggregates, but generated an acceptable performance of columns when 1–2-μm C18 silica beads were employed. To operate columns of 53 mm × 4.6 mm I.D., the maximum flow-rate needs to be ca. 2.5 ml/min …
Lipid hydroperoxides determination in milk‐based infant formulae by gas chromatography
2003
A simple gas chromatograph using a flame ionization detector and a polar capillary column method is proposed for determining hydroperoxides in the lipid fraction of milkbased infant formulas. Tricosanoic acid is used as internal standard. The method includes the following steps: a) the extraction of fat with chloroform/methanol (2:1, v/v), b) the reduction of hydroperoxide acids to hydroxide acids with hydrogen gas and palladium as a catalyst, c) the transmethylation to obtain the methyl esters with acetyl chloride and methanol/ hexane (4:1, v/v), and d) an acetylation with acetic anhydride/ pyridine (4:1, v/v) to obtain an acetoxy derivate of the hydroxide present. Two chromatography runs,…