The residual contents of fluoroquinolones in fish and shrimp were analyzed by using HPLC-FLD and LC-MS. The limit of detection (LOD) and limit of quantification (LOQ) for fluoroquinolones by HPLC-FLD were 0.0030-0.0083 and 0.0090-0.0252 mg/kg, respectively. Those by LC-MS were 0.0019-0.0040 and 0.0059-0.0122 mg/kg, respectively. Recoveries regarding ofloxacin, norfloxacin, pefloxacin, ciprofloxacin and enrofloxacin ranged from 76.4-104.6%. The detection rate of fluoroquinolones was 7.5% from a total of 268 samples. In only one Korean bullhead sample, the sum of ciprofloxacin and enrofloxacin contents was detected at a higher level than its maximum residue limits (MRL) of 0.1 mg/kg. Ofloxacin, norfloxacin and pefloxacin were not detected in any samples and detection rates of ciprofloxacin and enrofloxacin were 3.4% and 6.7%, respectively. In detection rate by species eel (2.6%), loach (2.2%), Korean bullhead (1.5%), carp (0.7%) and snakehead (0.4%) were in order.
Diarrhetic shellfish poisoning toxins were investigated by liquid chromatography-electrospray ionization mass spectrometry (LC-MS/MS). Okadaic acid (OA), Dinophysistoxin-1 (DTX1), Pectonotoxin2, (PTX2) and Yessotoxin (YTX) in bivalves were quantified. OA were found in four samples; mussel Mytilus edulis (0.001 µg/g), Oyster Crassostrea gigas (0.004 and 0.001 µg/g) and manila clam Ruditapes philippinarum (0.001 µg/g). DTX1, PTX2, and YTX were not detected from all of the samples examined.
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