Multilaboratory validation of a method to confirm chloramphenicol in shrimp and crabmeat by liquid chromatography-tandem mass spectrometry.
An existing method for chloramphenicol (CAP) determination in shrimp using a gas chromatograph with electron capture detector was adapted for confirmation of CAP with a liquid chromatograph interfaced to a triple quadrupole mass spectrometer. CAP residues are extracted from tissue with ethyl acetate, isolated via liquid-liquid extraction, and concentrated by evaporation. Extracts are chromatographed by using a reversed-phased column and analyzed by electrospray negative mode tandem mass spectrometry. Four product ions (m/z 152, 176, 194, and 257) of precursor m/z 321 were monitored. Moving from gas chromatography to liquid chromatography-tandem mass spectrometry improved the sensitivity of the method greatly, enabling reliable confirmation of CAP residues at 0.3 microg/kg (ppb). The method meets confirmation criteria recommended by the U.S. Food and Drug Administration and 4-point identification criteria established by the European Union. With slight modifications to accommodate different equipment, the method was validated in 3 laboratories.
Hammack
Walter
W
Florida Department of Agriculture and Consumer Services, Chemical Residue Laboratory, 3125 Conner Blvd, Tallahassee, FL 32399, USA.
Carson
Mary C
MC
Neuhaus
Barbara K
BK
Hurlbut
Jeffrey A
JA
Nochetto
Cristina
C
Stuart
James S
JS
Brown
Amy
A
Kilpatrick
Donna
D
Youngs
Kristl
K
Ferbos
Krystle
K
Heller
David N
DN
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D003386:Brachyura / Q000737:chemistry*; D002498:Centrifugation; D002701:Chloramphenicol / Q000032:analysis*; D002853:Chromatography, Liquid; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D008460:Meat / Q000032:analysis*; D033561:Penaeidae / Q000737:chemistry*; D015203:Reproducibility of Results; D012758:Shellfish / Q000032:analysis*; D012997:Solvents; D014481:United States; D014486:United States Food and Drug Administration
D000900:Anti-Bacterial Agents; D007202:Indicators and Reagents; D012997:Solvents; D002701:Chloramphenicol