Confirmation of Phenylbutazone Residues in Bovine Kidney by Liquid Chromatography/Mass Spectrometry
| Autor: | Gene J Nandrea, Susan B. Clark, Mark R. Madson, Sherri B Turnipseed, Jeffrey A Hurlbut, John N. Sofos |
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| Rok vydání: | 2002 |
| Předmět: |
Pharmacology
Electrospray Chromatography Elution Ether Mass spectrometry Analytical Chemistry Ammonium hydroxide chemistry.chemical_compound chemistry Liquid chromatography–mass spectrometry Phenylbutazone medicine Environmental Chemistry Agronomy and Crop Science Quadrupole mass analyzer Food Science medicine.drug |
| Zdroj: | Journal of AOAC INTERNATIONAL. 85:1009-1014 |
| ISSN: | 1944-7922 1060-3271 |
| DOI: | 10.1093/jaoac/85.5.1009 |
| Popis: | A confirmatory method is described for phenylbutazone (PB) residues in bovine kidney tissue. Ground kidney tissue is diluted with water, and the mixture is made basic with 25% ammonium hydroxide in water; the lipids are extracted with ethyl and petroleum ethers. The ether layer is discarded, and the tissue is acidified with 6N HCl. PB residues are extracted with tetrahydrofuran–hexane (1 + 4). The extract is passed through a silica solid-phase extraction column, and the eluate is evaporated to dryness. The residue is dissolved in acidified acetonitrile–water–acetic acid (50 + 49.4 + 0.6). A single quadrupole mass spectrometer coupled to a liquid chromatograph with an electrospray interface is used to confirm the identity of the PB residues in the kidney extract. Negative-ion detection with selected-ion monitoring of 4 ions is used. Sets of control and fortified-control kidney tissues (at 50, 100, and 200 ppb PB) and several kidney tissue field samples were analyzed for method validation. The method was tested further during the course of a survey to determine the incidence of PB residues in bovine kidney samples obtained from slaughterhouses across the country. In addition, the method was tested for use with an ion-trap mass spectrometer coupled to a liquid chromatograph, which allowed confirmation of PB at lower levels (5–10 ppb) in kidney tissue. |
| Databáze: | OpenAIRE |
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