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 (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.
Kubala-Drincic
Helena
H
Department of Residue Analysis, Croatian Veterinary Institute, 143 Savska Street, HR-10000 Zagreb, Croatia. helena.kubala-drincic@zg.hinet.hr
Bazulic
Davorin
D
Sapunar-Postruznik
Jasenka
J
Grubelic
Mirela
M
Stuhne
Goran
G
D000818:Animals; D000900:Anti-Bacterial Agents; D002417:Cattle; D002701:Chloramphenicol / Q000032:analysis*; D002849:Chromatography, Gas / Q000379:methods*; D005506:Food Contamination; D018482:Muscle, Skeletal / Q000737:chemistry*; D011200:Poultry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013552:Swine
D000900:Anti-Bacterial Agents; D002701:Chloramphenicol