PMID- 8823929
OWN - NLM
STAT- MEDLINE
DCOM- 19961202
LR  - 20191210
IS  - 1060-3271 (Print)
IS  - 1060-3271 (Linking)
VI  - 79
IP  - 5
DP  - 1996 Sep-Oct
TI  - Determination and confirmation of identities of flumequine and nalidixic, 
      oxolinic, and piromidic acids in salmon and shrimp.
PG  - 1227-35
AB  - A previously published liquid chromatographic (LC) method for determining 
      residues of flumequine (FLU) and nalidixic (NAL), oxolinic (OXO), and piromidic 
      (PIR) acids in catfish tissue was applied to salmon and shrimp muscle. Identities 
      of all 4 residues in salmon and shrimp were confirmed by gas chromatography/mass 
      spectrometry (GC/MS). The tissue is homogenized with acetone, the acetone extract 
      is defatted with hexane, and the quinolones are extracted into chloroform. The 
      extract is further purified by first partitioning into base and then 
      back-extracting from a solution acidified to pH 6.0. Analytes are determined by 
      LC with simultaneous UV and fluorescence detection. Muscle tissue was fortified 
      with each quinolone at 5, 10, 20, 40, and 80 ng/g. Average recoveries and 
      relative standard deviations (RSDs) for salmon, which represent an average of the 
      5 levels for each analyte, ranged from 75.9 to 90.8% and from 2.25 to 6.40%, 
      respectively. Average recoveries and RSDs for shrimp ranged from 81.3 to 91.2% 
      and from 7.34 to 10.7%, respectively. Identities of OXO, FLU, NAL, and PIR were 
      confirmed in extracts of salmon and shrimp tissue fortified at 10 ng/g by 
      determination of decarboxylated quinolones by GC/MS. Four diagnostic ions were 
      monitored for OXO, FLU, and PIR, and 5 ions were monitored for NAL. All ion 
      relative abundances were within 10% of those calculated for standard 
      decarboxylated quinolones. Optimum conditions for decarboxylation and GC/MS 
      confirmation are given.
FAU - Pfenning, A P
AU  - Pfenning AP
AD  - U.S. Food and Drug Administration, Animal Drugs Research Center, Denver, CO, USA.
FAU - Munns, R K
AU  - Munns RK
FAU - Turnipseed, S B
AU  - Turnipseed SB
FAU - Roybal, J E
AU  - Roybal JE
FAU - Holland, D C
AU  - Holland DC
FAU - Long, A R
AU  - Long AR
FAU - Plakas, S M
AU  - Plakas SM
LA  - eng
PT  - Journal Article
PL  - England
TA  - J AOAC Int
JT  - Journal of AOAC International
JID - 9215446
RN  - 0 (Anti-Infective Agents)
RN  - 0 (Fluoroquinolones)
RN  - 0 (Quinolizines)
RN  - 3B91HWA56M (Nalidixic Acid)
RN  - 3I12WH4EWF (Piromidic Acid)
RN  - L0A22B22FT (Oxolinic Acid)
RN  - UVG8VSP2SJ (flumequine)
SB  - IM
MH  - Animals
MH  - Anti-Infective Agents/*analysis/metabolism
MH  - Decapoda/*metabolism
MH  - Drug Residues/*analysis/metabolism
MH  - *Fluoroquinolones
MH  - Food Contamination
MH  - Gas Chromatography-Mass Spectrometry
MH  - Muscles/chemistry/metabolism
MH  - Nalidixic Acid/analysis/metabolism
MH  - Oxolinic Acid/analysis/metabolism
MH  - Piromidic Acid/analysis/metabolism
MH  - Quinolizines/analysis/metabolism
MH  - Reference Standards
MH  - Salmon/*metabolism
EDAT- 1996/09/01 00:00
MHDA- 1996/09/01 00:01
CRDT- 1996/09/01 00:00
PHST- 1996/09/01 00:00 [pubmed]
PHST- 1996/09/01 00:01 [medline]
PHST- 1996/09/01 00:00 [entrez]
PST - ppublish
SO  - J AOAC Int. 1996 Sep-Oct;79(5):1227-35.