High-throughput quantitative analysis of domoic acid directly from mussel tissue using Laser Ablation Electrospray Ionization – tandem mass spectrometry

Beach, Daniel G.; Walsh, Callee M.; McCarron, Pearse

doi:10.1016/j.toxicon.2014.10.009

Cited by 29 publications

(20 citation statements)

References 23 publications

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“…Laser-based techniques such as laser assisted electrospray ionization (LAESI) MSI [12] and transmission geometry laser ablation MSI [13] are relatively recent developments. Both methods involve the ablation of analytes from the sample using a laser followed by ionization via ESI mechanics, and they are able to generate spatial resolutions on biological surfaces of around 30 [14] and 50 µm, respectively, with LAESI also being able to perform high throughput quantitative analysis on biological samples [15]. Spray-based techniques such as DESI MSI rely on the use of a pneumatically directed electrospray mist to desorb and ionize analytes on surfaces [16].…”

Section: Introductionmentioning

confidence: 99%

High-Resolution Ambient MS Imaging of Negative Ions in Positive Ion Mode: Using Dicationic Reagents with the Single-Probe

Rao

Pan

Tian

et al. 2015

J. Am. Soc. Mass Spectrom.

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We have used the Single-probe, a miniaturized sampling device utilizing in-situ surface microextraction for ambient mass spectrometry (MS) analysis, for the high resolution MS imaging (MSI) of negatively charged species in the positive ionization mode. Two dicationic compounds, 1,5-pentanediyl-bis(1-butylpyrrolidinium) difluoride [C5(bpyr)2F2] and 1,3-propanediyl-bis(tripropylphosphonium) difluoride [C3(triprp)2F2], were added into the sampling solvent to form 1+ charged adducts with the negatively charged species extracted from tissues. We were able to detect 526 and 322 negatively charged species this way using [C5(bpyr)2F2] and [C3(triprp)2F2], respectively, including oleic acid, arachidonic acid, and several species of phosphatidic acid, phosphoethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, and others. In conjunction with the identification of the non-adduct cations, we have tentatively identified a total number of 1200 and 828 metabolites from mouse brain sections using [C5(bpyr)2F2] and [C3(triprp)2F2], respectively, through high mass accuracy measurements (mass error <5 ppm); MS/MS analyses were also performed to verify the identity of selected species. In addition to the high mass accuracy measurement, we were able to generate high spatial resolution (~17 µm) MS images of mouse brain sections. Our study demonstrated that utilization of dicationic compounds in the surface microextraction with the Single-probe device can perform high mass and spatial resolution ambient MSI measurements of broader types of compounds in tissues. Other reagents can be potentially used with the Single-probe device for a variety of reactive MSI studies to enable the analysis of species that are previously intractable.

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Section: Introductionmentioning

confidence: 99%

High-Resolution Ambient MS Imaging of Negative Ions in Positive Ion Mode: Using Dicationic Reagents with the Single-Probe

Rao

Pan

Tian

et al. 2015

J. Am. Soc. Mass Spectrom.

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“…TOF enables accurate molecular weight (MW) to be determined, allowing for exact MW match suitable for non-target analysis. In light of the most LC-MS requirement for extensive extraction and clean-up for complicated matrices, the use of laser ablation electrospray ionization (LAESI) with MS/MS could further eliminate sample extraction or clean-up so that DA in mussel tissue homogenates can be directly detected with a detection limit of 1 mg/kg, and recovery of 103-125% [75]. Combined with the use of NMR, many new algal toxins have been identified and their structures have been characterized in the recent years.…”

Section: Recent Development In Instrumental Analysis Of Algal Toxinsmentioning

confidence: 99%

Current Techniques for Detecting and Monitoring Algal Toxins and Causative Harmful Algal Blooms

2014

J Environ Anal Chem

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The detection and monitoring techniques for algal toxins and the causative harmful algal blooms (HABs) are essential for the protection of aquatic lives, shellfish safety, drinking water quality, and public health. Toward the development of fast, easy, and reliable techniques, much progress has been made during the last decade for the qualitative and quantitative analysis of algal toxins. This review highlights the recent progress and new trends of these analytical and monitoring tools, ranging from in-situ quick screening protocols for the monitoring of algal blooms to mass spectrometric analysis of trace levels of various algal toxins and structural elucidation. Solid-phase adsorption toxin tracking (SPATT) deployed in the field for the passive sampling of algal toxins has been recently validated, and improved ELISA-based methods with lower detection limits for more toxins have become commercially available for both screening and routine monitoring purposes. Liquid chromatography-mass spectrometry with several recent mass spectrometric innovations has expanded our understanding of traditional toxins, their metabolites along with newly discovered toxins of ecological importance. Several established in vivo and in vitro bioassays will continue to be used as benchmark toxicological testing of algal toxins; however, newly emerged molecular probing techniques such as real-time quantitative polymerase chain reaction (qPCR) have extended our ability to trace algal toxins from causative organisms at the molecular level. New chemical and biological sensors, lab-on-chip and remote sensing of blooms being developed will hold promise for early warning and routine monitoring to better manage and protect our freshwater, coastal and marine resources from adverse impact by harmful algal blooms.

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“…The majority of applications of LAESI have focused on mass spectrometry imaging of plant and animal tissues, but it has also been used for direct targeted and non‐targeted analysis in liquid samples and biological specimens . To date, the capability of LAESI‐MS for targeted quantitative analysis directly from complex samples has remained largely unexplored . Recently, we proposed that LAESI‐MS/MS could be used as a high‐throughput method for quantitative DA analysis and showed detection of DA directly from shellfish tissue homogenates .…”

mentioning

confidence: 99%

“…To date, the capability of LAESI‐MS for targeted quantitative analysis directly from complex samples has remained largely unexplored . Recently, we proposed that LAESI‐MS/MS could be used as a high‐throughput method for quantitative DA analysis and showed detection of DA directly from shellfish tissue homogenates . This preliminary proof of concept work considered only the blue mussel ( Mytilus edulus ) and only analyzed DA standards, spiked tissue and mussel tissue matrix reference materials.…”

mentioning

confidence: 99%

“…Here, as a follow‐up to our original communication, we investigate the suitability of LAESI‐MS for analysis of DA in a wide range of real shellfish samples previously analyzed for DA in a regulatory setting. The first goal of this project was to refine the LAESI‐MS method for DA in shellfish tissue homogenates compared with the previous work, including transfer of the original method to a high‐resolution mass spectrometer for improved selectivity and sensitivity. Various sample preparation approaches and LAESI‐MS parameters were also optimized, with respect to the sensitivity of analysis, reproducibility and matrix effects.…”

mentioning

confidence: 99%

See 1 more Smart Citation

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

Beach

Walsh²,

Cantrell³

et al. 2016

Rapid Comm Mass Spectrometry

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RationaleDomoic 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.MethodsWe 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.ResultsDomoic 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.ConclusionsThese 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.

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High-throughput quantitative analysis of domoic acid directly from mussel tissue using Laser Ablation Electrospray Ionization – tandem mass spectrometry

Cited by 29 publications

References 23 publications

High-Resolution Ambient MS Imaging of Negative Ions in Positive Ion Mode: Using Dicationic Reagents with the Single-Probe

High-Resolution Ambient MS Imaging of Negative Ions in Positive Ion Mode: Using Dicationic Reagents with the Single-Probe

Current Techniques for Detecting and Monitoring Algal Toxins and Causative Harmful Algal Blooms

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

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