MULTI-RESIDUE CONFIRMATION OF AMINOGLYCOSIDE ANTIBIOTICS AND BOVINE KIDNEY BY ION-SPRAY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY TANDEM MASS-SPECTROMETRY
Lg. Mclaughlin et al., MULTI-RESIDUE CONFIRMATION OF AMINOGLYCOSIDE ANTIBIOTICS AND BOVINE KIDNEY BY ION-SPRAY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY TANDEM MASS-SPECTROMETRY, Biological mass spectrometry, 23(7), 1994, pp. 417-429
An ion spray high-performance liquid chromatographic/tandem mass spect
rometric (HPLC/MS/MS) method capable of determining the following six
aminoglycosides in bovine kidney is presented: spectinomycin, hygromyc
in B, streptomycin, dihydrostreptomycin, gentamicin C complex and neom
ycin B. Tobramycin was used as an internal standard. This method uses
an improved matrix solid-phase dispersion (MSPD) method for tissue ext
raction. A gradient HPLC separation was developed with mobile phases c
onsisting of aqueous 20 mM pentafluoropropionic acid and acetonitrile.
Protonated molecules served as precursor ions for collision-induced d
issociation (CID) and three product ions were chosen for each analyte
for selected reaction monitoring (SRM) where possible. A validation st
udy was conducted for the confirmation of dihydrostreptomycin, neomyci
n B and four major components of the gentamicin C complex through SRM
HPLC/MS/MS analysis of negative control, fortified and incurred bovine
kidney samples. All of the samples analyzed could be confirmed with i
on ratios within 15% of the daily mean of fortified standards and 90%
of the samples had ion ratios within 10%. All compounds except spectin
omycin could be detected (while monitoring three ions by SRM) in bovin
e kidney tissue at or below the regulatory level of concern. MSPD reco
veries were aceptable with the exception of the 27% value observed for
spectinomycin.