PMID- 17475272
OWN - NLM
STAT- MEDLINE
DCOM- 20070906
LR  - 20191210
IS  - 0021-9673 (Print)
IS  - 0021-9673 (Linking)
VI  - 1154
IP  - 1-2
DP  - 2007 Jun 22
TI  - Development of a pressurised liquid extraction and liquid chromatography with 
      electrospray ionization-tandem mass spectrometry method for the determination of 
      domoic acid in shellfish.
PG  - 287-94
AB  - Amnesic shellfish poisoning (ASP) is a potentially lethal human toxic syndrome 
      which is caused by domoic acid (DA) that originates in marine phytoplankton 
      belonging to the Pseudonitzschia genus. A confirmatory and sensitive procedure 
      has been developed and validated for the determination of DA in shellfish. The 
      proposed method includes pressurised liquid extraction (PLE) with 
      methanol/acetone (9:1), florisil clean-up purification inside the PLE extraction 
      cell and detection by liquid chromatography (LC) coupled to electrospray 
      ionization in positive mode tandem mass spectrometry (ESI-MS-MS). Comparison of 
      ionization sources (ESI, atmospheric pressure ionization (APCI) atmospheric 
      pressure photoionization (APPI) and combined APCI/APPI) were carried out in order 
      to improve the analytical signal. The main parameters affecting the performance 
      of the different ionization sources and PLE parameters were previously optimised 
      using statistical design of experiments (DOE). Linear calibrations were obtained 
      using mussel tissue extracts 0.05-5 microg DA/ml (R2>0.999). The limits of 
      detection (LOD) and quantitation (LOQ) of the method were 0.2 and 0.5 microg/g 
      respectively and recoveries ranged from 81 to 95%. This method was successfully 
      applied to determine DA levels in 46 shellfish samples collected from Valencian 
      (Spain) supermarkets, showing high sample throughput.
FAU - Pardo, Olga
AU  - Pardo O
AD  - Public Health Laboratory of Valencia, Conselleria de Sanitat, Cami de la Marjal, 
      s/n 46470 Albal, Valencia, Spain.
FAU - Yusa, Vicent
AU  - Yusa V
FAU - Leon, Nuria
AU  - Leon N
FAU - Pastor, Agustin
AU  - Pastor A
LA  - eng
PT  - Journal Article
PT  - Validation Study
DEP - 20070404
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - M02525818H (domoic acid)
RN  - SIV03811UC (Kainic Acid)
SB  - IM
MH  - Animals
MH  - Chromatography, Liquid/*methods
MH  - Kainic Acid/*analogs & derivatives/analysis
MH  - Sensitivity and Specificity
MH  - Shellfish/*analysis
MH  - Spectrometry, Mass, Electrospray Ionization/*methods
MH  - Tandem Mass Spectrometry/*methods
EDAT- 2007/05/04 09:00
MHDA- 2007/09/07 09:00
CRDT- 2007/05/04 09:00
PHST- 2006/12/17 00:00 [received]
PHST- 2007/03/27 00:00 [revised]
PHST- 2007/03/30 00:00 [accepted]
PHST- 2007/05/04 09:00 [pubmed]
PHST- 2007/09/07 09:00 [medline]
PHST- 2007/05/04 09:00 [entrez]
AID - S0021-9673(07)00630-9 [pii]
AID - 10.1016/j.chroma.2007.03.118 [doi]
PST - ppublish
SO  - J Chromatogr A. 2007 Jun 22;1154(1-2):287-94. doi: 10.1016/j.chroma.2007.03.118. 
      Epub 2007 Apr 4.