Screening of sulphonamides in egg using gas chromatography-mass-selective detection and liquid chromatography-mass spectrometry.
A rapid extraction and clean-up procedure for sulphonamide antibiotics in eggs suitable for both GC-MSD and LC-MS end determinations has been developed. The drugs were extracted using acetonitrile, acidified using acetic acid and cleaned-up using cation- and anion-exchange. For determination by GC-MSD, extracts were derivatised with diazomethane followed by pentafluoropropionic acid anhydride. For LC-MS extracts were taken up in water and used directly. The methodology developed was validated at the 100 and 25 microg kg(-1) levels, equivalent to the MRL and one quarter of the MRL. Results for the GC-MS procedure were quantitated against deuterated sulphadiazine with relative recoveries ranging from 54% for sulphachloropyridazine to 135.5% for sulphamethazine. Recoveries for the LC-MS procedure ranged from 33% for sulphaguanidine to 92% for sulphamethazine and sulphadimethoxine.
Ministry of Agriculture, Fisheries and Food, Central Science Laboratory, Sand Hutton, York, UK.
J A
JA
Tarbin
P
P
Clarke
G
G
Shearer
D002853:Chromatography, Liquid / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D010063:Ovum / Q000737:chemistry*; D012015:Reference Standards; D013449:Sulfonamides / Q000032:analysis*
D013449:Sulfonamides