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Matrix solid-phase dispersion extraction and gas chromatographic determination of chloramphenicol in muscle tissue.

作者信息

Kubala-Drincic Helena, Bazulic Davorin, Sapunar-Postruznik Jasenka, Grubelic Mirela, Stuhne Goran

机构信息

Department of Residue Analysis, Croatian Veterinary Institute, 143 Savska Street, HR-10000 Zagreb, Croatia.

出版信息

J Agric Food Chem. 2003 Feb 12;51(4):871-5. doi: 10.1021/jf025939d.

Abstract

A method based on matrix solid-phase dispersion (MSPD) was developed for the gas chromatographic (GC) determination of chloramphenicol (CAP) residues in animal muscle tissue. Muscle tissue was blended with octadecylsilyl-derivatized silica (C(18)). A column made from the C(18)/muscle tissue matrix was washed with n-hexane and acetonitrile/water (5 + 95), after which CAP was eluted with acetonitrile/water (50 + 50) and partitioned into ethyl acetate. The final extract was evaporated, and a trimethylsilyl derivative of CAP was prepared with Sylon HTP and detected by GC with an electron capture detector (ECD) and a mass spectrometer. For quantitation, the internal standard used was the meta isomer of CAP (m-CAP) for GC-ECD. Muscle tissue samples were fortified at three concentration levels. At 5, 10, and 15 microg/kg levels the respective mean recoveries were 93, 96, and 98%, and the repeatabilities were 13, 11, and 3%. The detection and quantitation limits with ECD were 1.6 and 4.0 microg/kg, respectively. No statistically significant difference was observed in the efficiency of CAP extraction from muscle tissue of various animals (bovine, porcine, and poultry) by the MSPD technique.

摘要

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