The determination of melamine in muscle tissue by liquid chromatography/tandem mass spectrometry
- 27 November 2007
- journal article
- research article
- Published by Wiley in Rapid Communications in Mass Spectrometry
- Vol. 21 (24), 4027-4032
- https://doi.org/10.1002/rcm.3289
Abstract
In early 2007 it was determined that the compound melamine, suspected of having been involved in the deaths of numerous pets, had been fed to hogs intended for human consumption. This report describes a method for the analysis of melamine in porcine muscle tissue using solid‐phase extraction (SPE) and high‐performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Melamine was extracted in 50% acetonitrile in water. Homogenates were centrifuged and supernatants were acidified and washed with methylene chloride. The aqueous extracts were cleaned up using mixed‐mode C8/strong cation exchange SPE and then concentrated, fortified with a stable isotope‐labeled analog of melamine, and analyzed by HPLC/MS/MS. Gradient HPLC separation was performed using an ether‐linked phenyl column with ammonium acetate/acetic acid and acetonitrile as the mobile phase. Multiple reaction monitoring (MRM) mode of two precursor‐product ion transitions for melamine and one for the internal standard was used. A five point calibration curve ranging from 50 to 2000 ng/mL of melamine in solvent was used to establish instrument response. The method was validated by analysis of seven replicate porcine muscle tissue samples fortified with 10 ng/g of melamine. The mean recovery for the seven replicates was 83% with 6.5% relative standard deviation and the calculated method detection limit was 1.7 ng/g. Copyright © 2007 John Wiley & Sons, Ltd.Keywords
This publication has 11 references indexed in Scilit:
- Analysis of melamine resins by capillary zone electrophoresis with electrospray ionization‐mass spectrometric detectionElectrophoresis, 2005
- Residue determination of cyromazine and its metabolite melamine in chard samples by ion-pair liquid chromatography coupled to electrospray tandem mass spectrometryAnalytica Chimica Acta, 2004
- Analytical Method for the Determination of Cyromazine and Melamine Residues in Soil Using LC-UV and GC-MSDJournal of Agricultural and Food Chemistry, 2000
- The Fragmentation of Melamine: A Study via Electron-Impact Ionization, Laser-Desorption Ionization, Collision-Induced Dissociation, and Density Functional Calculations of Potential Energy SurfaceThe Journal of Physical Chemistry B, 1998
- Development of Improved Immunoassay and HPLC Methods for the Analysis of Chlorodiamino-s-triazine in Environmental SamplesJournal of Agricultural and Food Chemistry, 1996
- Stability of Plastics Monomers in Food-Simulating Liquids under European Union Migration Test ConditionsJournal of Agricultural and Food Chemistry, 1994
- Determination of melamine and three hydrolytic products by liquid chromatographyBulletin of Environmental Contamination and Toxicology, 1990
- Capillary gas chromatographic separation and mass spectrometric detection of cyromazine and its metabolite melamineJournal of Chromatography A, 1987
- Urolithiasis and bladder carcinogenicity of melamine in rodentsToxicology and Applied Pharmacology, 1984
- Determination of seventeen s-triazine herbicides and derivatives by high-pressure liquid chromatographyJournal of Agricultural and Food Chemistry, 1981