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.
The concentration of quinoxaline-2-carboxylic acid (QCA) determined by HPLC after alkaline hydrolysis of liver and muscle of swine, ranged from < 3 ng/g to 45.3 ng/g in liver, and from < 3 ng/g to 10.8 ng/g in muscle samples. After the 77th day of therapy QCA was found in samples of liver (9.7 ng/g). Recoveries obtained for both liver and muscle were 70% at 5 ng/g, 77% and 75% respectively at 10 ng/g, and 90% for both liver and muscle at 30 ng/g. This experiment was performed within the frame of the National Monitoring Programme of Residues in Animal Tissues in the Republic of Croatia.
The aim of this study was to assess the suitability of the perirenal fatty tissue for the determination of an organochlorine pesticide. Fatty tissue samples were prepared by the matrix solid phase dispersion (MSPD) method, and pesticide levels were determined by gas chromatography on capillary column using an electron capture detector. Results were confirmed by gas chromatography/mass spectrometry (GC/MS) system. The results showed that the perirenal fatty tissue contained significantly higher levels of hexachlorobenzene (HCB) than the dorsal fatty tissue (P < 0.01). All the levels were below the criteria for maximum residue limits established by Croatia and the EU.
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