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Veterinary Drug Residues Subgroup

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Veterinary Drug Residues Subgroup
Veterinary Drug Residues Subgroup
Report for 2010 AOAC
Chemical Contaminants & Residues
in Food Community
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Call for seafood methods
Call for methods
Drug Residues in Shrimp, Catfish, Tilapia, and Salmon
“Validated multi-residue method(s) for select veterinary drug residues
using high technology in shrimp, catfish, tilapia, and salmon has been
identified as method(s) that are most urgently needed. AOAC
INTERNATIONAL is inviting method authors to submit your method to
AOAC for consideration and evaluation through the AOAC Official
Methods program.”
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Call for seafood methods
Drug residues of interest:
Drug Residues
Examples
Analytical Range
(µg/g or ppb)
Nitrofuran marker
residues
SEM, AHD, AMOZ, AOZ
1.0-3.6
Chloramphenicol
0.3-1.2
Fluoroquinolones
Ciprofloxacin, enrofloxacin,
sarafloxacin
1.0-3.6
Quinolones
Oxolinic acid, flumequine,
naladixic acid
0.5-2.0
Dyes
Malachite green, crystal violet,
leuco forms
1.0-3.6
Methyltestosterone
0.8-3.0
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Response to call for methods
In response to this call, there were over 20 submissions:
• 5 for fluoroquinolones and quinolones
• 5 for phenicols (chloramphenicol)
• 6 for dyes
• 5 for nitrofurans
• 0 for methyltestosterone
• 4 multiclass multiresidue methods
 Methods submitted from state, federal, private labs
 Methods from 10 different countries to be evaluated
 Several other applicable methods found in the literature
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Subgroup to evaluate methods
Subgroup meeting tomorrow (Tuesday)
from 1:15 – 3:45 PM
• Evaluate seafood methods
• Recommend 2-3 methods of each type (multi, NFs, etc.)
• Identify potential study directors and participating labs
• Discussion may be continued via WebEx
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Subgroup to evaluate methods
Methods have been summarized:
Title
From
Extraction/Clean-up
Detection
Detection Limits
Recoveries(RSDs)
Other Comments
Multiresidue method for the
triphenylmethane dyes in
fish: MG, CV, and BG
(catfish, trout, basa,
tilapia, salmon, shrimp)
FDA
DEN/
ADRC
Extract w/ ammonium acetate
buffer (pH 4.5) + ACN, (HAH, pTSA) (2x)
LLE w/ DCM and H2O (2x)
DDQ oxidation (leuco --> dye)
SPE (Alumina N + PRS, stacked, 1
step)
LC & LC-MS/MS
LC:C18 ; ACN/
AmmAc
VIS:620 (MG); 588
(GV)
LC-MS :
LC: PH ; ACN/0.1%F
MS : ND-APCI+, MS2
LODs: 0.1-0.2 ppb
LOQs: 0.2-0.5 ppb
> 86% (11%) MG
> 91% (11%) CV
67% (15%) BG
Validation: n
>30/cmpd
+ incurred samples
Cmpds:LMG+MG,
LCV+CV, BG
Quant:-external stds
(VIS)
Confirm: MS2 spectra
• Summary tables will be available at the subgroup meeting.
• Copies of full submissions will also be available.
• Subgroup attendees will need to sign confidentiality agreement.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Other AOAC business relating to veterinary drugs
Expert Review Panels (ERPs):
 2009: Under contract with Elanco Animal Health, an AOAC ERP
met to evaluate methods for tylosin, tilmicosin, narasin, monensin,
and ractopamine in animal tissue.
 2010: Contract was extended to nicarbazin, avilamycin, and
apramycin. A call for methods has been issued, and another ERP
will meet to evaluate procedures for these drug residues.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Recent trends in vet drug residue methods
 Multiclass multiresidue methods
 Streamlined sample preparation
 Accurate mass LC-MS
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Multiclass multiresidue methods
Examples of recent publications:
Multiclass, multiresidue drug analysis, including
aminoglycosides, in animal tissue using LC coupled to tandem
MS Martos et al., J. Agric. Food Chem. 2010, 58, 5932.
Multiclass, multiresidue method for the detection of antibiotic
residues in distillers grains by LC and ion trap tandem MS. De
Alwis & Heller, J. Chromatogr. A 2010, 1217, 3076.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Streamlined sample preparation: QuEChERS
Examples of recent publications:
 Development of fast screening methods for the analysis of
veterinary drug residues in milk by LC-triple quadrupole MS.
Vidal, et al., Anal. Bioanal. Chem. 2010, 397, 2777.
 The development and validation of a multiclass liquid
chromatography tandem LC-MS/MS procedure for the
determination of veterinary drug residues in animal tissue
using a QuEChERS approach. Stubbings & Bigwood, Anal. Chim.
Acta 2009, 637, 68.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Streamlined sample prep: On-line SPE
Examples of recent publications:
 Fully automated screening of veterinary drugs in milk by
turbulent flow chromatography and tandem MS. Stolker, et al.,
Anal. Bioanal. Chem. 2010, 397, 2841.
 High-throughput screening for multi-class veterinary drug
residues in animal muscle using LC/tandem MS with on-line
solid-phase extraction. Tang, et al., Rapid Commun. Mass
Spectrom. 2006, 20, 2565.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Accurate mass LC-MS



Targeted & non-targeted analytes
TOF, Q-TOF
Orbitrap
Several symposia at the meeting feature this topic
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Accurate mass LC-MS
Examples of recent publications:
 Multi-residue screening of veterinary drugs in egg, fish and meat using
high resolution LC accurate mass TOF MS. Peters, et al., J. Chromatogr. A
2009, 1216, 8206.
 Comprehensive fast multiresidue screening of 150 veterinary drugs in
milk by UHPLC coupled to TOF MS. Ortelli, et al., J. Chromatogr. B 2009,
877, 2363.
 Full-Scan accurate Mass Selectivity of UHPLC Combined with TOF and
Orbitrap MS in Hormone and Veterinary Drug Residue Analysis. van der
Heeft, et al., J. Amer. Soc. Mass Spectrom. 2009, 20, 451.
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
Veterinary Drug Residues Subgroup
Reminder:
Subgroup meeting tomorrow (Tuesday)
from 1:15 – 3:45 PM
• Evaluate seafood methods
• Any other issues members want to discuss
124th AOAC Annual Meeting & Exposition
September 26-29, 2010
Loews Royal Pacific Resort at Universal Orlando • Orlando, Florida
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