PMID- 16001850
OWN - NLM
STAT- MEDLINE
DCOM- 20050919
LR  - 20211203
IS  - 1060-3271 (Print)
IS  - 1060-3271 (Linking)
VI  - 88
IP  - 3
DP  - 2005 May-Jun
TI  - Multiresidue method for determination of algal toxins in shellfish: 
      single-laboratory validation and interlaboratory study.
PG  - 761-72
AB  - A method that uses liquid chromatography with tandem mass spectrometry (LC/MS/MS) 
      has been developed for the highly sensitive and specific determination of amnesic 
      shellfish poisoning toxins, diarrhetic shellfish poisoning toxins, and other 
      lipophilic algal toxins and metabolites in shellfish. The method was subjected to 
      a full single-laboratory validation and a limited interlaboratory study. Tissue 
      homogenates are blended with methanol-water (9 + 1), and the centrifuged extract 
      is cleaned up with a hexane wash. LC/MS/MS (triple quadrupole) is used for 
      quantitative analysis with reversed-phase gradient elution (acidic buffer), 
      electrospray ionization (positive and negative ion switching), and 
      multiple-reaction monitoring. Ester forms of dinophysis toxins are detected as 
      the parent toxins after hydrolysis of the methanolic extract. The method is 
      quantitative for 6 key toxins when reference standards are available: 
      azaspiracid-1 (AZA1), domoic acid (DA), gymnodimine (GYM), okadaic acid (OA), 
      pectenotoxin-2 (PTX2), and yessotoxin (YTX). Relative response factors are used 
      to estimate the concentrations of other toxins: azaspiracid-2 and -3 (AZA2 and 
      AZA3), dinophysis toxin-1 and -2 (DTX1 and DTX2), other pectenotoxins (PTX1, 
      PTX6, and PTX11), pectenotoxin secoacid metabolites (PTX2-SA and PTX11-SA) and 
      their 7-epimers, spirolides, and homoYTX and YTX metabolites (45-OHYTX and 
      carboxyYTX). Validation data have been gathered for Greenshell mussel, Pacific 
      oyster, cockle, and scallop roe via fortification and natural contamination. For 
      the 6 key toxins at fortification levels of 0.05-0.20 mg/kg, recoveries were 
      71-99% and single laboratory reproducibilities, relative standard deviations 
      (RSDs), were 10-24%. Limits of detection were <0.02 mg/kg. Extractability data 
      were also obtained for several toxins by using successive extractions of 
      naturally contaminated mussel samples. A preliminary interlaboratory study was 
      conducted with a set of toxin standards and 4 mussel extracts. The data sets from 
      8 laboratories for the 6 key toxins plus DTX1 and DTX2 gave within-laboratories 
      repeatability (RSD(R)) of 8-12%, except for PTX-2. Between-laboratories 
      reproducibility (RSDR) values were compared with the Horwitz criterion and ranged 
      from good to adequate for 7 key toxins (HorRat values of 0.8-2.0).
FAU - McNabb, Paul
AU  - McNabb P
AD  - Cawthron Institute, 98 Halifax St E, Nelson, New Zealand.
FAU - Selwood, Andrew I
AU  - Selwood AI
FAU - Holland, Patrick T
AU  - Holland PT
FAU - Aasen, J
AU  - Aasen J
FAU - Aune, T
AU  - Aune T
FAU - Eaglesham, G
AU  - Eaglesham G
FAU - Hess, P
AU  - Hess P
FAU - Igarishi, M
AU  - Igarishi M
FAU - Quilliam, M
AU  - Quilliam M
FAU - Slattery, D
AU  - Slattery D
FAU - Van de Riet, J
AU  - Van de Riet J
FAU - Van Egmond, H
AU  - Van Egmond H
FAU - Van den Top, H
AU  - Van den Top H
FAU - Yasumoto, T
AU  - Yasumoto T
LA  - eng
PT  - Journal Article
PL  - England
TA  - J AOAC Int
JT  - Journal of AOAC International
JID - 9215446
RN  - 0 (Ethers, Cyclic)
RN  - 0 (Furans)
RN  - 0 (Heterocyclic Compounds, 3-Ring)
RN  - 0 (Hydrocarbons, Cyclic)
RN  - 0 (Imines)
RN  - 0 (Macrolides)
RN  - 0 (Marine Toxins)
RN  - 0 (Mollusk Venoms)
RN  - 0 (Oxocins)
RN  - 0 (Pyrans)
RN  - 0 (Spiro Compounds)
RN  - 0 (Toxins, Biological)
RN  - 0 (azaspiracid)
RN  - 0 (pectenotoxin 6)
RN  - 1W21G5Q4N2 (Okadaic Acid)
RN  - 4Q51CVY9O2 (dinophysistoxin 1)
RN  - 54NE3O7Z3A (pectenotoxin 1)
RN  - 7TV3J97IT8 (gymnodimine)
RN  - 97564-91-5 (pectenotoxin 2)
RN  - M02525818H (domoic acid)
RN  - P6M9FM2L2G (yessotoxin)
RN  - RH78DHY1JZ (dinophysistoxin 2)
RN  - SIV03811UC (Kainic Acid)
RN  - Y4S76JWI15 (Methanol)
SB  - IM
MH  - Animals
MH  - Biological Assay
MH  - Chromatography, Liquid/*methods
MH  - Ethers, Cyclic/analysis
MH  - Food Analysis/*methods
MH  - Furans/analysis/metabolism
MH  - Heterocyclic Compounds, 3-Ring/analysis
MH  - Hydrocarbons, Cyclic/analysis
MH  - Hydrolysis
MH  - Imines/analysis
MH  - Kainic Acid/analogs & derivatives/analysis
MH  - Macrolides
MH  - Marine Toxins/analysis
MH  - Mass Spectrometry/*methods
MH  - Methanol/chemistry
MH  - Mice
MH  - Mollusca
MH  - Mollusk Venoms
MH  - Okadaic Acid/analysis
MH  - Oxocins/analysis
MH  - Pyrans/analysis/metabolism
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
MH  - Shellfish
MH  - Spiro Compounds/analysis
MH  - Time Factors
MH  - Toxins, Biological/*analysis
EDAT- 2005/07/09 09:00
MHDA- 2005/09/20 09:00
CRDT- 2005/07/09 09:00
PHST- 2005/07/09 09:00 [pubmed]
PHST- 2005/09/20 09:00 [medline]
PHST- 2005/07/09 09:00 [entrez]
PST - ppublish
SO  - J AOAC Int. 2005 May-Jun;88(3):761-72.