engleski

Matrix Solid-Phase Dispersion Extraction and Gas Chromatographic Determination of Chloramphenicol in Muscle Tissue

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 (C18). A column made from C18/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.

chloramphenicol; gas chromatography; matrix solid-phase dispersion; muscle tissue; residues

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