PMID- 17394125
OWN - NLM
STAT- MEDLINE
DCOM- 20070607
LR  - 20191210
IS  - 0951-4198 (Print)
IS  - 0951-4198 (Linking)
VI  - 21
IP  - 9
DP  - 2007
TI  - Determination of tetracycline antibiotics in cow's milk by liquid 
      chromatography/tandem mass spectrometry.
PG  - 1511-20
AB  - A liquid chromatographic/tandem mass spectrometric (LC/MS/MS) multiresidue method 
      for the simultaneous quantitative determination of oxytetracycline, 
      4-epi-oxytetracycline, tetracycline, 4-epi-tetracycline, chlortetracycline, 
      4-epi-chlortetracycline and doxycycline in milk has been developed. An extraction 
      procedure consisting of a liquid extraction of the milk samples with 
      trichloroacetic acid was performed. The extract was centrifuged and the 
      supernatant was filtered. Solid-phase extraction (SPE) with an OASIS HLB SPE 
      column was used to clean up the sample extracts. The samples were analysed by 
      LC/MS/MS. The LC separation was performed on a reversed-phase C18 column using 
      gradient elution with a mobile phase consisting of water and a mixture of 
      methanol/acetonitrile. The tetracycline analytes were detected with a quadrupole 
      mass spectrometer using positive ion electrospray ionisation. The confirmatory 
      method has acceptable detection limits and the different tetracyclines can be 
      detected at a residue concentration between 5 and 20 microg/L. The method is 
      validated according to the European requirements for veterinary drug residues and 
      all determined parameters were found to conform to the criteria. The recovery 
      values ranged from 90.4 to 101.2% with relative standard deviations (RSDs) no 
      larger than 9.7%. The overall or between-day precision of the analytical assay 
      determined as repeatability at several residue concentrations and expressed as 
      RSD ranged from 3.3 to 10%. This analytical assay is a useful tool within the 
      Belgian monitoring programme for confirmation of samples which have been 
      positively screened for residues of tetracyclines in raw farm cow's milk.
CI  - Copyright 2007 John Wiley & Sons, Ltd.
FAU - De Ruyck, Hendrik
AU  - De Ruyck H
AD  - Institute for Agricultural and Fisheries Research (ILVO), Technology and Food 
      Unit (T&V), Food Safety, Brusselsesteenweg 370, 9090 Melle, Belgium. 
      Hendrik.Deruyck@ilvo.vlaanderen.be
FAU - De Ridder, Herman
AU  - De Ridder H
LA  - eng
PT  - Journal Article
PT  - Validation Study
PL  - England
TA  - Rapid Commun Mass Spectrom
JT  - Rapid communications in mass spectrometry : RCM
JID - 8802365
RN  - 0 (Anti-Bacterial Agents)
RN  - 0 (Tetracyclines)
SB  - IM
MH  - Animals
MH  - Anti-Bacterial Agents/*analysis/chemistry
MH  - *Chromatography, High Pressure Liquid
MH  - Milk/*chemistry
MH  - Spectrometry, Mass, Electrospray Ionization/*methods
MH  - Tandem Mass Spectrometry/*methods
MH  - Tetracyclines/*analysis/chemistry
EDAT- 2007/03/31 09:00
MHDA- 2007/06/08 09:00
CRDT- 2007/03/31 09:00
PHST- 2007/03/31 09:00 [pubmed]
PHST- 2007/06/08 09:00 [medline]
PHST- 2007/03/31 09:00 [entrez]
AID - 10.1002/rcm.2991 [doi]
PST - ppublish
SO  - Rapid Commun Mass Spectrom. 2007;21(9):1511-20. doi: 10.1002/rcm.2991.