Search results for "Detection limit"
showing 10 items of 810 documents
Flow injection biamperometric determination of chloramphenicol and related nitro compounds by on-line chemical photodegradation
2000
Abstract An unsegmented continuous-flow assembly for the determination of chloramphenicol is proposed. The determination is based on the on-line photodegradation of the drug in an NH4+/NH3 buffer at pH 10.4 by using a photoreactor consisting of a 697 cm long × 0.8 mm ID piece of PTFE tubing coiled around an 8 W low-pressure mercury lamp. Photodegraded chloramphenicol is detected by photolytic cleavage of nitrite from the parent compound as well as by organic oxidizing photofragments, and their subsequent reaction with iodide ion, which is monitored biamperometrically. Triiodide thus formed is detected in excess iodide solution by polarizing two platinum electrodes at 100 mV. The calibration…
Gas chromatographic behaviour of urea herbicides
2001
Gas chromatographic conditions for determining eight phenylurea (chlortoluron, diuron, fluometuron, isoproturon, linuron, metabenzthiazuron, metobromuron and monuron) and one sulfonylurea (chlorsulfuron) herbicides were assessed. Degradation products of the herbicides formed in the injector were used for identification. Most phenylureas formed their respective carbamic acid methyl esters, metabenzthiazuron formed an aminobenzothiazol and chlorsulfuron formed an aminotriazine plus a phenylsulfonamide. On-column injection of standards using a BP10 capillary column was evaluated to identify the chromatographic behaviour. Detection limits ranged from 0.05 ng for chlorsulfuron to 3 ng for monuro…
First-order derivative resolution of overlapped PAH peaks with common mass spectra in gas chromatography–mass spectrometry
2007
Abstract First-order derivative of 15 points smoothed chromatograms of mixtures of benzo( b )fluoranthene (BbF) and benzo( k )fluoranthene (BkF) for the m / z 252 ion obtained using two microscans has been proposed as a simple alternative to the resolution of overlapped chromatographic peaks of these two compounds which have identical mass spectra. The procedure provides limits of detection of 12 and 29 ng g −1 for BbF and BkF, respectively and offers the possibility to use the 250 and 248 ions to confirm the identity of these analytes.
Liquid chromatographic determination of trimethylamine in water.
2004
A method for the selective determination of trimethylamine (TMA) in aqueous matrices by liquid chromatography is reported. The proposed procedure is based on the derivatization of the analyte with 9-fluorenylmethyl chloroformate (FMOC) in a precolumn (Hypersil C18, 30 microm, 20 mm x 2.1 mm i.d.) connected on-line to the analytical column (LiChrosphere 100 RP18, 5 microm, 125 mm x 4 mm i.d.). Gradient elution was performed with a mixture of acetonitrile-water-0.05 M borate buffer (pH 9.0). The method has been applied to the direct determination of TMA in water within the 0.25-10.0 microg/ml concentration interval, and can also be adapted to the determination of TMA over the range 0.05-1.0 m…
Rapid whole protein quantification of staphylococcal enterotoxin B by liquid chromatography
2012
Abstract Food poisoning caused by Staphylococcus aureus is one of the most important foodborne diseases in the world. The ability of these bacteria to produce one or more enterotoxins in milk and dairy products is linked to staphylococcal food poisoning. Enterotoxin B (SEB) is an exotoxin produced by S. aureus and is one of the compounds most frequently involved in staphylococcal food poisoning worldwide. In this work, 20 samples of milk collected from restaurants have been studied for the presence of S. aureus enterotoxigenic strains. All the isolates from milk samples have been analysed by liquid chromatography-coupled with diode array detector for the rapid identification and quantificat…
Comparative assessment of three extraction procedures for determination of emerging Fusarium mycotoxins in pasta by LC–MS/MS
2013
Abstract A new rapid, sensitive, reproducible and reliable method was developed for the quantitative determination of enniatins A, A1, B and B1, beauvericin and fusaproliferin in dry and fresh pasta by liquid chromatography-triple quadrupole-tandem mass spectrometry. A comparative study of different rapid and economical extraction procedures was performed for the extraction of these mycotoxins in pasta. For this purpose, three different approaches were studied during the extraction step (Ultra-Turrax, ultrasonic bath and microwave). Optimal extraction conditions were reached using Ultra-Turrax with acetonitrile for 3 min without purification step. The chromatographic separation of the six m…
Contributions to the analysis of organic xenobiotics in fish
1995
For the residue-analysis of fish samples, a method has been developed to separate the medium polar triazines and acetamides together with lipophilic xenobiotics (organochlorine pesticides, PCBs and octachlorostyrene) from fish tissue. The detection limits of the analytes are mostly within the ppt-range (ng/kg fillet) and vary between 40 and 1050 ng/kg fillet of fish. Their recoveries range from 75 to 108%, spiked at 1.5 μg/kg. The substances are extracted with a mixture of petroleum ether/ethylacetate (2:1) using a soxhlet apparatus. Subsequently, the lipids in the sample extracts are reduced to 0.4% by gel chromatography. A 5 g silica gel clean-up separates the analytes according to their …
Comparison of different methods for extraction of polycyclic aromatic hydrocarbons (PAHs) from Sicilian (Italy) coastal area sediments.
2012
This paper describes a work aimed at improving the conditions of an extraction method, coupling GC-MS determination, for the analysis without cleanup phase, of polycyclic aromatic hydrocarbons (PAHs) from sediment samples. The automatic Soxhlet extraction in warm mode (using Extraction System B-811 Standard, Buchi) has demonstrated advantages for automation, reduced extraction time, and lower solvent use than for conventional Soxhlet extraction. Under these conditions, the recoveries are very good as they resulted greater than 85 % and, in most of the cases, near 100 %. The repeatability is also satisfactory (relative standard deviation less than 15 %). The detection limits are also accepta…
Improvement of the electrophoretic protein profiles of Leguminosae gums extracts using gamanase and application to the evaluation of carob–guar mixtu…
2004
Abstract A quantitative assay for guar gum in carob gum, based on the extraction of proteins in acetonitrile–water (7:3), separation by capillary electrophoresis and multiple linear regression (MLR) using the areas of nine selected peaks as predictors, was improved by performing the extraction in the presence of gamanase. In the absence of the enzyme, peak migration times and areas depended on the guar content, which complicated peak identification and evaluation. Manual correction of the migration times by comparison with standard electropherograms obtained with pure carob and carob–guar mixtures was required; however, when the proteins were extracted under sonication at 60 °C for 30 min i…
Determination of -Ascorbic Acid in Lycopersicon Fruits by Capillary Zone Electrophoresis
2001
This study shows an improved method for the determination of L-ascorbic acid (l-AA) in fruits of Lycopersicon by capillary zone electrophoresis (CZE). Two backgrounds electrolytes (BGEs) have been tested: (i) 400 mM borate at pH 8.0 and 1 x 10(-2)% hexadimethrine bromide, for the separation of Eulycopersicon subgenus species; and (ii) as in BGE(i) but supplemented with 20% (v/v) acetonitrile, for the separation of species of the Eriopersicon subgenus. The present procedures were compared with two routine methods-enzymatic assay and potentiometric titration with 2,6-dichlorophenol-indophenol. While these routine methods presented some difficulties in quantifying l-AA in several Lycopersicon …