PMID- 12772270
OWN - NLM
STAT- MEDLINE
DCOM- 20030716
LR  - 20131121
IS  - 0951-4198 (Print)
IS  - 0951-4198 (Linking)
VI  - 17
IP  - 11
DP  - 2003
TI  - Confirmatory analysis of sulfonamide antibacterials in bovine liver and kidney: 
      extraction with hot water and liquid chromatography coupled to a single- or 
      triple-quadrupole mass spectrometer.
PG  - 1146-56
AB  - A simple, specific, and rapid confirmatory method for determining 12 sulfonamide 
      (SAs) antibacterials in bovine liver and kidney is presented. This method is 
      based on the matrix solid-phase dispersion technique with hot water as extractant 
      followed by liquid chromatography/mass spectrometry (LC/MS) with an electrospray 
      ion source. The method was tailored for use with both single-quadrupole MS (I) 
      and triple-quadrupole MS (II) instruments. After acidification and filtration of 
      the aqueous extract, a 250-microL aliquot was injected into instrument I while 
      only 25 microL was analyzed by instrument II. With instrument I MS data 
      acquisition was performed in the selected ion monitoring (SIM) mode, selecting at 
      least three ions for each target compound. With instrument II the selected 
      reaction monitoring (SRM) mode with three fragmentation reactions for each 
      compound was chosen. With the exception of sulfaquinoxaline (SQX), recovery of 
      the analytes at the 50 ppb level in both liver and kidney was 72-96% with 
      relative standard deviations (RSDs) ranging between 3 and 11%. The very poor 
      recovery of SQX was due to its rapid enzymatic oxidation when in contact with the 
      two tissues. With instrument I, limits of quantification (LOQs, S/N = 10) were 
      5-14 ppb of SAs. Even lower LOQs (1-8 ppb) were estimated by using instrument II, 
      even though the extract volume analyzed was ten times lower than that with 
      instrument I. With both matrices and using instrument I, severe ion signal 
      suppression was experienced for the early-eluted SAs when trying to fractionate 
      analytes by using a short chromatographic run time. This effect was traced to 
      polar endogenous co-extractives eluted in the first part of the chromatographic 
      run that interfered with gas-phase ion formation for SAs. Adopting more selective 
      chromatographic conditions minimized this effect.
CI  - Copyright 2003 John Wiley & Sons, Ltd.
FAU - Bogialli, Sara
AU  - Bogialli S
AD  - Dipartimento di Chimica, Universita "La Sapienza", Piazza Aldo Moro 5, 00185 
      Roma, Italy.
FAU - Curini, Roberta
AU  - Curini R
FAU - Di Corcia, Antonio
AU  - Di Corcia A
FAU - Nazzari, Manuela
AU  - Nazzari M
FAU - Sergi, Manuel
AU  - Sergi M
LA  - eng
PT  - Journal Article
PL  - England
TA  - Rapid Commun Mass Spectrom
JT  - Rapid communications in mass spectrometry : RCM
JID - 8802365
RN  - 0 (Anti-Bacterial Agents)
RN  - 0 (Sulfonamides)
RN  - 0 (Tissue Extracts)
RN  - 059QF0KO0R (Water)
SB  - IM
MH  - Animals
MH  - Anti-Bacterial Agents/chemistry/*pharmacokinetics
MH  - Cattle
MH  - Chromatography, Liquid
MH  - Drug Residues/pharmacokinetics
MH  - Hot Temperature
MH  - Kidney/*metabolism
MH  - Liver/*metabolism
MH  - Mass Spectrometry/*methods
MH  - Molecular Structure
MH  - Sulfonamides/chemistry/*pharmacokinetics
MH  - Tissue Extracts
MH  - Water/*chemistry
EDAT- 2003/05/29 05:00
MHDA- 2003/07/17 05:00
CRDT- 2003/05/29 05:00
PHST- 2003/05/29 05:00 [pubmed]
PHST- 2003/07/17 05:00 [medline]
PHST- 2003/05/29 05:00 [entrez]
AID - 10.1002/rcm.1031 [doi]
PST - ppublish
SO  - Rapid Commun Mass Spectrom. 2003;17(11):1146-56. doi: 10.1002/rcm.1031.