PMID- 20186537
OWN - NLM
STAT- MEDLINE
DCOM- 20100426
LR  - 20211020
IS  - 1618-2650 (Electronic)
IS  - 1618-2642 (Print)
IS  - 1618-2642 (Linking)
VI  - 396
IP  - 8
DP  - 2010 Apr
TI  - Quantitative analysis of penicillins in porcine tissues, milk and animal feed 
      using derivatisation with piperidine and stable isotope dilution liquid 
      chromatography tandem mass spectrometry.
PG  - 3027-40
LID - 10.1007/s00216-010-3523-0 [doi]
AB  - Penicillins are used universally in both human and veterinary medicine. The 
      European Union (EU) has established maximum residue levels (MRLs) for most 
      ss-lactam antibiotics in milk and animal tissues and included them in the 
      National Residue Monitoring Programs. In this study, a novel method is described 
      for the determination and confirmation of eight penicillins in porcine tissues, 
      milk and animal feed by liquid chromatography-tandem mass spectrometry 
      (LC-MS/MS). To prevent degradation of penicillin residues during workup, a 
      derivatisation procedure was developed, by which penicillins were converted to 
      stable piperidine derivatives. Deuterated piperidine derivatives were synthesised 
      for all relevant penicillins, enabling the use of isotope dilution for accurate 
      quantification. Penicillin residues were derivatised in the crude extract with 
      piperidine and isolated using solid-phase extraction. The penicillin piperidine 
      derivatives were determined by LC-MS/MS. The method was validated at the current 
      MRLs, which range from 25-300 microg kg(-1) in muscle and kidney to 4-30 microg 
      kg(-1) in milk as well as at the target value of 100 microg kg(-1) chosen for 
      animal feed, according to the EU requirements for a quantitative confirmatory 
      method. Accuracy ranged from 94-113% (muscle), 83-111% (kidney) and 87-103% 
      (milk) to 88-116% (animal feed). Intra-day precision (relative standard deviation 
      (RSD)(r)) ranged from 5-13% (muscle, n = 18), 4-17% (kidney, n = 7) and 5-18% 
      (milk, n = 7) to 11-32% (animal feed, n = 18). Inter-day precision (RSD(RL), n = 
      18) ranged from 6-23% (muscle) to 11-36% (animal feed). From the results, it was 
      concluded that the method was fit for purpose at the target MRLs in animal tissue 
      and target levels for animal feed.
FAU - van Holthoon, Frederique
AU  - van Holthoon F
AD  - RIKILT-Institute of Food Safety, Wageningen UR, Akkermaalsbos 2, P.O. Box 230, 
      6700 AE Wageningen, The Netherlands.
FAU - Mulder, Patrick P J
AU  - Mulder PP
FAU - van Bennekom, Eric O
AU  - van Bennekom EO
FAU - Heskamp, Henri
AU  - Heskamp H
FAU - Zuidema, Tina
AU  - Zuidema T
FAU - van Rhijn, Hans J A
AU  - van Rhijn HJ
LA  - eng
PT  - Journal Article
DEP - 20100226
PL  - Germany
TA  - Anal Bioanal Chem
JT  - Analytical and bioanalytical chemistry
JID - 101134327
RN  - 0 (Penicillins)
RN  - 0 (Piperidines)
RN  - 0 (Protons)
RN  - 67I85E138Y (piperidine)
SB  - IM
MH  - Animal Feed/*analysis
MH  - Animals
MH  - Chromatography, Liquid/instrumentation/*methods
MH  - Indicator Dilution Techniques
MH  - Kidney/*chemistry
MH  - Milk/*chemistry
MH  - Molecular Structure
MH  - Muscle, Skeletal/*chemistry
MH  - Penicillins/*analysis/chemistry
MH  - Piperidines/chemistry
MH  - Protons
MH  - Swine
MH  - Tandem Mass Spectrometry/instrumentation/*methods
PMC - PMC2844525
EDAT- 2010/02/27 06:00
MHDA- 2010/04/27 06:00
PMCR- 2010/02/26
CRDT- 2010/02/27 06:00
PHST- 2009/11/16 00:00 [received]
PHST- 2010/02/01 00:00 [accepted]
PHST- 2010/01/26 00:00 [revised]
PHST- 2010/02/27 06:00 [entrez]
PHST- 2010/02/27 06:00 [pubmed]
PHST- 2010/04/27 06:00 [medline]
PHST- 2010/02/26 00:00 [pmc-release]
AID - 3523 [pii]
AID - 10.1007/s00216-010-3523-0 [doi]
PST - ppublish
SO  - Anal Bioanal Chem. 2010 Apr;396(8):3027-40. doi: 10.1007/s00216-010-3523-0. Epub 
      2010 Feb 26.