Laser ablation electrospray ionization high-resolution mass spectrometry for regulatory screening of domoic acid in shellfish

Rationale Domoic acid (DA) is a potent neurotoxin that accumulates in shellfish. Routine testing involves homogenization, extraction and chromatographic analysis, with a run time of up to 30 min. Improving throughput using ambient ionization for direct analysis of DA in tissue would result in signif...

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Bibliographic Details
Published in:Rapid communications in mass spectrometry 2016-11, Vol.30 (22), p.2379-2387
Main Authors: Beach, Daniel G., Walsh, Callee M., Cantrell, Pamela, Rourke, Wade, O'Brien, Sinead, Reeves, Kelley, McCarron, Pearse
Format: Article
Language:English
Subjects:
Animals
Government regulations
Homogenizing
Ionization
Kainic Acid - analogs & derivatives
Kainic Acid - analysis
Kainic Acid - chemistry
Laser ablation
Lasers
Marine Toxins - analysis
Marine Toxins - chemistry
Mass spectrometry
Reproducibility of Results
Routines
Screening
Shellfish
Shellfish - analysis
Shellfish - standards
Spectrometry, Mass, Electrospray Ionization - methods
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Summary:Rationale Domoic acid (DA) is a potent neurotoxin that accumulates in shellfish. Routine testing involves homogenization, extraction and chromatographic analysis, with a run time of up to 30 min. Improving throughput using ambient ionization for direct analysis of DA in tissue would result in significant time savings for regulatory testing labs. Methods We assess the suitability of laser ablation electrospray ionization high‐resolution mass spectrometry (LAESI‐HRMS) for high‐throughput screening or quantitation of DA in a variety of shellfish matrices. The method was first optimized for use with HRMS detection. Challenges such as tissue sub‐sampling, isobaric interferences and method calibration were considered and practical solutions developed. Samples included 189 real shellfish samples previously analyzed by regulatory labs as well as mussel matrix certified reference materials. Results Domoic acid was selectively analyzed directly from shellfish tissue homogenates with a run time of 12 s. The limits of detection were between 0.24 and 1.6 mg DA kg−1 tissue, similar to those of LC/UV methods. The precision was between 27 and 44% relative standard deviation (RSD), making the technique more suited to screening than direct quantitation. LAESI‐MS showed good agreement with LC/UV and LC/MS and was capable of identifying samples above and below 5 mg DA kg−1 wet shellfish tissue, one quarter of the regulatory limit. Conclusions These findings demonstrate the suitability of LAESI‐MS for routine, high‐throughput screening of DA. This approach could result in significant time savings for regulatory labs carrying out shellfish safety testing on thousands of samples annually. © 2016 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd.
ISSN:0951-4198
1097-0231
DOI:10.1002/rcm.7725