Search results for "Liquid Chromatography"
showing 10 items of 942 documents
Development and validation of a pressurized liquid extraction liquid chromatography–tandem mass spectrometry method for perfluorinated compounds dete…
2009
Abstract This paper describes the development and validation of an analytical methodology to determine eight perfluorinated compounds (PFCs) in edible fish using pressurized liquid extraction (PLE) with water and solid-phase extraction (SPE) with an ion-exchanger as extraction and pre-concentration procedures, followed by liquid chromatography–quadrupole-linear ion trap mass spectrometry (LC–QqLIT–MS). The rapidity and effectiveness of the proposed extraction procedure were compared with those most commonly used to isolate PFCs from fish (ion-pairing and alkaline digestion). The average recoveries of the different fish samples, spiked with the eight PFCs at three levels (the LOQ, 10 and 100…
HPLC: a tool for the analysis of T-2 toxin and HT-2 toxin in cereals.
1984
An analytical procedure for the determination of trichothecenes in various cereals is described. HPLC was performed with a reversed-phase (C18) column eluted with methanol:water (60:40, v/v). Compounds were detected with a refractive index detector. The elution patterns of free and contaminated samples were compared. The recovery of added T-2 toxin (2 and 5 micrograms/g) in rye and wheat was approximately 80%. The application of this method allows for combined use with other sensitive methods such as mass spectrometry and gas chromatography. The described method is operationally simple, relatively inexpensive, and requires no derivatization.
Isolation of oligopeptides from the water-soluble extract of goat cheese and their identification by mass spectrometry
2001
A procedure for the separation and identification of small peptides from the water-soluble fraction of a goat cheese was developed. The water-soluble extract was ultrafiltered (1000 Da membrane cutoff), and peptides were isolated by sequential chromatography: size exclusion chromatography (HPLC-grade water), anion exchange chromatography (phosphate buffer gradient), and semipreparative reverse-phase high-performance liquid chromatography (water/acetonitrile gradient). The fractions obtained were analyzed by combined mass spectrometry methods including electrospray ionization, liquid secondary ionization, and tandem mass spectrometry to identify and to confirm the sequences of 28 tri- to oct…
Determination of carbosulfan and its metabolites in oranges by liquid chromatography ion-trap triple-stage mass spectrometry.
2005
Liquid chromatography ion-trap mass spectrometry LC-MSn has been successfully applied to identify and confirm carbosulfan and seven of its metabolites in oranges after pressurized liquid extraction (PLE) with dichloromethane. Mass spectra of carbosulfan and its metabolites were investigated using multiple stages of mass spectrometry. Although interpretation of the fragmentation pathways, based on mass spectra, enables structural elucidation and identification of these compounds, the proposed fragmentation pathways and ion structures need verification by exact mass measurements. The analytical method--PLE and LC-MS3 --was validated: limits of quantification (LOQ) ranged from 0.01 to 0.07 mg …
Determination of bisphenol diglycidyl ether residues in canned foods by pressurized liquid extraction and liquid chromatography–tandem mass spectrome…
2005
Abstract A new confirmatory method for simultaneous determination of bisphenol diglycidyl ether residues (BADGE, BADGE·H2O, BADGE·2H2O, BADGE·H2O·HCl, BADGE·HCl, BADGE·2HCl, BFDGE and BFDGE·2HCl) from canned food has been developed. The proposed method includes extraction by pressurized liquid extraction (PLE) followed by liquid–liquid partition and purification by solid phase extraction (SPE). Several solvent systems and different operating conditions (time, temperature) have been investigated for PLE optimization. A reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to atmospheric pressure chemical ionisation tandem mass spectrometry (APCI-MS–MS) method was developed …
Comparison of solid-phase microextraction and stir bar sorptive extraction for determining six organophosphorus insecticides in honey by liquid chrom…
2004
Abstract Two approaches based on sorptive extraction, solid-phase microextraction (SPME) and stir bar sorptive extraction (SBSE), in combination with liquid chromatography (LC)–atmospheric pressure chemical ionization mass spectrometry (MS) have been assayed for analyzing chlorpyriphos methyl, diazinon, fonofos, phenthoate, phosalone, and pirimiphos ethyl in honey. In both, SPME and SBSE, enrichment was performed using a poly(dimethylsiloxane) coating. Significant parameters affecting sorption process such as sample volume, sorption and desorption times, ionic strength, elution solvent, and dilution (water/honey) proportion were optimized and discussed. Performance of both methods has been …
Pesticide residue determination in fruit and vegetables by liquid chromatography–mass spectrometry
2000
An overview is given of pesticide residue determination in fruit and vegetables by liquid chromatography-mass spectrometry (LC-MS). Emphasis is placed on the thermospray, particle beam and atmospheric pressure ionization interfaces including advantages and drawbacks and typical detection limits. The capacity of each interface to provide useful data for identification/confirmation of analytes and the possibility of obtaining structural information for the identification of target and non-target compounds is discussed. Finally, sample preparation techniques are dealt with in relation to their influence on further LC-MS determination.
The expanding role of LC-MS in analyzing metabolites and degradation products of food contaminants
2008
Abstract Liquid chromatography-mass spectrometry (LC-MS) has contributed significantly in advancing research in the analysis of metabolites and degradation products of food contaminants. Of particular interest is the comprehensive application of LC-MS to discovery of degradation products and metabolites. This review, covering research published between 2003 and 2008, describes how LC-MS has been used in this field, with the majority of work dealing with target-metabolite analysis and only a small fraction using LC-MS comprehensively. In considering the significance of this topic and the potential interest in it, we briefly describe state-of-the art mass analyzers applied for it (QtrAP, QqTO…
Über polygermane
1986
Abstract The synthesis of GePh4 and Ge2Ph6 by Grignard reaction in THF or ether/toluene leads to the by-products Ge3Ph8 (up to 11%) and Ge4Ph10 (up to 18%) which is dependant on using an excess of Mg. A quantitative analysis of the resulting products by HPLC and a semipreparative separation by column, flash, and HPL chromatography is described. The crystal structures of Ge3Ph8 (R = 0.075) and Ge4Ph10 · 2C6H6 (R = 0.054) have been determined. Ge4Ph10 has Ci symmetry and both chain conformations are well staggered (49–70° for Ge3Ph8, 53–66° for Ge4Ph10). The GeGe distances and GeGeGe angles are 244 pm and 121° (Ge3Ph8), and 246 pm and 118° (Ge4Ph10).