Gas-liquid chromatographic determination of nifursol in frozen turkey tissues to ten parts per billion.
Nifursol (3,5-dinitrosalicylic acid (5-nitrofurfurylidene) hydrazide) is extracted into ethyl acetate from 10 g tissue in the presence of sodium sulfate. Tissue interferences are removed from the tissue extract by washing with petroleum ether after the extract has been transferred into an aqueous solution by evaporation of ethyl acetate. The drug is hydrolyzed under acid conditions to form 5-nitro-2-furaldehyde (5NF). After partition of 5NF from the aqueous phase into benzene the extract is further cleaned up on a Florisil column. The 5NF is eluted from the Florisil column with benzeneethyl acetate. Electron capture gas-liquid chromatography of a 10 mul injection of the concentrated column eluate is the determinative step. Quantitation is accomplished by comparison of the peak height of the sample to the peak height of the standard which is carried through the method simultaneously. Studies of method performance on turkey muscle, liver, kidney, and skin tissues fortified to contain 10 ppb nifursol show a recovery range of 87.4-95.0% and a coefficent of variation range of 5.7-11.2%.
D000818:Animals; D002849:Chromatography, Gas; D003080:Cold Temperature; D007668:Kidney / Q000032:analysis; D008099:Liver / Q000032:analysis; D008722:Methods; D008832:Microchemistry; D009132:Muscles / Q000032:analysis; D009581:Nitrofurans / Q000032:analysis* / Q000378:metabolism; D010573:Pesticide Residues / Q000032:analysis; D012867:Skin / Q000032:analysis; D014422:Turkeys
D009581:Nitrofurans; D010573:Pesticide Residues