Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry

Domènech, Albert; Cortés-Francisco, Nuria; Palacios, Òscar; Franco, José M.; Riobó, Pilar; Llerena, José J; Vichi, Stefania; Caixach, Josep

doi:10.1016/j.chroma.2013.12.071

Cited by 50 publications

(35 citation statements)

References 20 publications

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“…Overall, standard deviations of the error were slightly lower on the Orbitrap (0.46 ppm) compared to the QToF (0.58 ppm). These results showed a good stability in mass measurement for both instruments and were consistent with previously published mass accuracy data [14,15]. For all toxins on all instruments, mean calibration curves obtained from triplicate injections of methanol, SPATT and mussel solutions showed good linearity (R 2 > 0.99) (see Supplementary material, Table S4).…”

Section: Methods Selection and Performancesupporting

confidence: 86%

“…In general the good detection limits obtained with HRMS for the other toxins illustrated the capacity for quantitative screening of toxins in comparison with more conventional LRMS approaches. The significant added advantage of HRMS is the ability to perform full scan and MS/MS acquisitions simultaneously [15,16], and thus enable retrospectively evaluation of data.…”

Section: Accuracy and Detection Limitsmentioning

confidence: 99%

“…This technique is now being increasingly used for monitoring [10,11] and for characterization of reference materials [12,13]. Additionally, methods using high resolution mass spectrometry (HRMS) have recently been developed and quantitatively validated for some marine toxins [14][15][16].…”

Section: Introductionmentioning

confidence: 99%

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High resolution mass spectrometry for quantitative analysis and untargeted screening of algal toxins in mussels and passive samplers

Zendong

McCarron

Herrenknecht

et al. 2015

Journal of Chromatography A

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Measurement of marine algal toxins has traditionally focussed on shellfish monitoring while, over the last decade, passive sampling has been introduced as a complementary tool for exploratory studies. Since 2011, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been adopted as the EU reference method (No. 15/2011) for detection and quantitation of lipophilic toxins. Traditional LC-MS approaches have been based on low-resolution mass spectrometry (LRMS), however, advances in instrument platforms have led to a heightened interest in the use of high-resolution mass spectrometry (HRMS) for toxin detection. This work describes the use of HRMS in combination with passive sampling as a progressive approach to marine algal toxin surveys. Experiments focused on comparison of LRMS and HRMS for determination of a broad range of toxins in shellfish and passive samplers. Matrix effects are an important issue to address in LC-MS; therefore, this phenomenon was evaluated for mussels (Mytilus galloprovincialis) and passive samplers using LRMS (triple quadrupole) and HRMS (quadrupole time-of-flight and Orbitrap) instruments. Matrix-matched calibration solutions containing okadaic acid and dinophysistoxins, pectenotoxin, azaspiracids, yessotoxins, domoic acid, pinnatoxins, gymnodimine A and 13-desmethyl spirolide C were prepared. Similar matrix effects were observed on all instruments types. Most notably, there was ion enhancement for pectenotoxins, okadaic acid/dinophysistoxins on one hand, and ion suppression for yessotoxins on the other. Interestingly, the ion selected for quantitation of PTX2 also influenced the magnitude of matrix effects, with the sodium adduct typically exhibiting less susceptibility to matrix effects than the ammonium adduct. As expected, mussel as a biological matrix, quantitatively produced significantly more matrix effects than passive sampler extracts, irrespective of toxin. Sample dilution was demonstrated as an effective measure to reduce matrix effects for all compounds, and was found to be particularly useful for the non-targeted approach. Limits of detection and method accuracy were comparable between the systems tested, demonstrating the applicability of HRMS as an effective tool for screening and quantitative analysis. HRMS offers the advantage of untargeted analysis, meaning that datasets can be retrospectively analyzed. HRMS (full scan) chromatograms of passive samplers yielded significantly less complex data sets than mussels, and were thus more easily screened for unknowns. Consequently, we recommend the use of HRMS in combination with passive sampling for studies investigating emerging or hitherto uncharacterized toxins.

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Section: Methods Selection and Performancesupporting

confidence: 86%

Section: Accuracy and Detection Limitsmentioning

confidence: 99%

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High resolution mass spectrometry for quantitative analysis and untargeted screening of algal toxins in mussels and passive samplers

Zendong

McCarron

Herrenknecht

et al. 2015

Journal of Chromatography A

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“…High resolution MS constitutes an alternative technique to determine the molecular mass, and provide structural data of phycotoxins and unknown bioactive molecules from toxic shellfish extracts with high accuracy and sensitivity. 131,132 However, when certified standards are not available, uncertainty – a parameter that provides an interval within which the true value is believed to lie at a set level of confidence – becomes difficult to estimate and the data are qualitative at best. 132 Total synthesis of CI toxins is of paramount importance for unambiguous detection and risk assessment.…”

Section: Current Methods For Detection Of CI Toxinsmentioning

confidence: 99%

Synthesis and biology of cyclic imine toxins, an emerging class of potent, globally distributed marine toxins

et al. 2015

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From a small group of exotic compounds isolated only two decades ago, Cyclic Imine (CI) toxins have become a major class of marine toxins with global distribution. Their distinct chemical structure, biological mechanism of action, and intricate chemistry ensures that CI toxins will continue to be the subject of fascinating fundamental studies in the broad fields of chemistry, chemical biology, and toxicology. The worldwide occurrence of potent CI toxins in marine environments, their accumulation in shellfish, and chemical stability are important considerations in assessing risk factors for human health. This review article aims to provide an account of chemistry, biology, and toxicology of CI toxins from their discovery to the present day.

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“…In recent years, these groups have been routinely monitored in shellfish using LC-MS/MS,based methods as proposed by the European Union Reference Laboratory for Marine Biotoxins (EURLMB). However, the use of full-scan high-resolution MS has recently been proposed as an alternative analytical platform for the quantitative measurement of marine lipophilic toxins in shellfish [23,24] and excellent validation data have been obtained with this methodology [25]. Indeed the quantitative performance of HR-Orbitrap MS has proved to be even better than MS/MS and excellent validation data have been obtained with this methodology [25].…”

Section: Introductionmentioning

confidence: 92%

Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry

et al. 2015

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During the last decade, a significant increase in the occurrence of harmful algal blooms (HABs), linked to repetitive cases of shellfish contamination has become a public health concern and therefore, accurate methods to detect marine toxins in different matrices are required. In this study, we developed a method for profiling lipophilic marine microalgal toxins based on ultra-high-performance liquid chromatography coupled to high-resolution Orbitrap mass spectrometry (UHPLC-HR-Orbitrap MS). Extraction of selected toxins (okadaic acid (OA), dinophysistoxin-1 (DTX-1), pectenotoxin-2 (PTX-2), azaspiracid-1 (AZA-1), yessotoxin (YTX) and 13-desmethyl spirolide C (SPX-1)) was optimized using a Plackett-Burman design. Three key algal species, i.e., Prorocentrum lima, Protoceratium reticulatum and Alexandrium ostenfeldii were used to test the extraction efficiency of OA, YTXs and SPXs, respectively. Prorocentrum micans, fortified with certified reference solutions, was used for recovery studies. The quantitative and confirmatory performance of the method was evaluated according to CD 2002/657/EC. Limits of detection and quantification ranged between 0.006 and 0.050 ng mL(-1) and 0.018 to 0.227 ng mL(-1), respectively. The intra-laboratory reproducibility ranged from 6.8 to 11.7 %, repeatability from 6.41 to 11.5 % and mean corrected recoveries from 81.9 to 119.6 %. In addition, algae cultures were retrospectively screened for analogues and metabolites through a homemade database. Using the ToxID software programme, 18 toxin derivates were detected in the extract of three toxin producing microalgae species. In conclusion, the generic extraction and full-scan HRMS approach offers an excellent quantitative performance and simultaneously allows to profile analogues and metabolites of marine toxins in microalgae. Graphical Abstract Optimization of extraction, detection and quantification of lipophilic marine toxins in microalgae by UHPLC-HR Orbitrap MS.

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Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry

Cited by 50 publications

References 20 publications

High resolution mass spectrometry for quantitative analysis and untargeted screening of algal toxins in mussels and passive samplers

High resolution mass spectrometry for quantitative analysis and untargeted screening of algal toxins in mussels and passive samplers

Synthesis and biology of cyclic imine toxins, an emerging class of potent, globally distributed marine toxins

Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry

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