Liquid Chromatography–Tandem Mass Spectrometry Method for the Screening of Eight Paralytic Shellfish Poisoning Toxins, Domoic Acid, 13-Desmethyl Spirolide C, Palytoxin and Okadaic Acid in Seawater

Carmela Riccardi, Francesca Buiarelli, Patrizia Di Filippo, Sisto Distratis, Luigi Giannetti, Maura Manganelli, Bruno Neri, Donatella Pomata, Mara Stefanelli

Research output: Contribution to journalArticle

Abstract

Abstract: A quick and reproducible screening analytical method for the simultaneous determination of algal toxins, belonging to different chemical classes, was developed to provide a toxin profile in seawater, useful to assess potential risks to environment and human health. The target compounds were: gonyautoxin-1,4, gonyautoxin-2,3, decarbamoylgonyautoxin-2,3, N‐sulfocarbamoyl-gonyautoxin-1,2, neosaxitoxin, decarbamoyl-neosaxitoxin, saxitoxin, decarbamoyl-saxitoxin, domoic acid, 13-desmethyl spirolide C (SPX1), palytoxin and okadaic acid. Extraction and clean-up were carried out with a combination of Bond Elut LRC-C18 and Carbograph4 cartridges connected in series. Analyte separation was performed in gradient elution mode in 12 min with a Gemini C18 column. Compound detection was carried out in multiple reaction monitoring and in positive ionization mode for paralytic shellfish poisoning toxins, domoic acid, SPX1 and palytoxin, and in negative ionization mode for okadaic acid. The toxins were quantified with matrix-matched calibration curves constructed by spiked seawater samples (concentration levels 0.02–2 μg L−1 depending on the compound). The method was reproducible with intra-day and inter-day relative standard deviations ranging from 4 to 9% and from 8 to 16%, respectively. Good recoveries (84–105%) and good accuracy (2–20%) were obtained by spiking experiments. Limits of detection were calculated for each toxin and varied from 0.011 to 0.12 μg L−1 depending on the compound. The developed method was applied to cultured Ostreopsis cf. ovata samples. The proposed procedure may be considered a valuable alternative to existing methods for monitoring toxic microalgae, since it offers a rapid screening of target toxins, reduced organic solvent consumption, and handling of smaller sample volumes while providing good sensitivity and accuracy. Graphical Abstract: [Figure not available: see fulltext.].

Original languageEnglish
Pages (from-to)277-288
Number of pages12
JournalChromatographia
Volume81
Issue number2
DOIs
Publication statusPublished - Feb 1 2018

Fingerprint

Shellfish Poisoning
Shellfish
Okadaic Acid
Seawater
Saxitoxin
Mass spectrometry
Mass Spectrometry
Screening
Ionization
Liquids
Monitoring
Poisons
Organic solvents
Microalgae
Health
Calibration
Recovery
Limit of Detection
domoic acid
gonyautoxins

Keywords

  • Algal toxins
  • Column liquid chromatography
  • Harmful algal blooms
  • Seawater samples
  • Solid-phase extraction

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Clinical Biochemistry
  • Organic Chemistry

Cite this

Liquid Chromatography–Tandem Mass Spectrometry Method for the Screening of Eight Paralytic Shellfish Poisoning Toxins, Domoic Acid, 13-Desmethyl Spirolide C, Palytoxin and Okadaic Acid in Seawater. / Riccardi, Carmela; Buiarelli, Francesca; Di Filippo, Patrizia; Distratis, Sisto; Giannetti, Luigi; Manganelli, Maura; Neri, Bruno; Pomata, Donatella; Stefanelli, Mara.

In: Chromatographia, Vol. 81, No. 2, 01.02.2018, p. 277-288.

Research output: Contribution to journalArticle

Riccardi, Carmela ; Buiarelli, Francesca ; Di Filippo, Patrizia ; Distratis, Sisto ; Giannetti, Luigi ; Manganelli, Maura ; Neri, Bruno ; Pomata, Donatella ; Stefanelli, Mara. / Liquid Chromatography–Tandem Mass Spectrometry Method for the Screening of Eight Paralytic Shellfish Poisoning Toxins, Domoic Acid, 13-Desmethyl Spirolide C, Palytoxin and Okadaic Acid in Seawater. In: Chromatographia. 2018 ; Vol. 81, No. 2. pp. 277-288.
@article{baf7a6e8386a44bf8ea968c6a67d0162,
title = "Liquid Chromatography–Tandem Mass Spectrometry Method for the Screening of Eight Paralytic Shellfish Poisoning Toxins, Domoic Acid, 13-Desmethyl Spirolide C, Palytoxin and Okadaic Acid in Seawater",
abstract = "Abstract: A quick and reproducible screening analytical method for the simultaneous determination of algal toxins, belonging to different chemical classes, was developed to provide a toxin profile in seawater, useful to assess potential risks to environment and human health. The target compounds were: gonyautoxin-1,4, gonyautoxin-2,3, decarbamoylgonyautoxin-2,3, N‐sulfocarbamoyl-gonyautoxin-1,2, neosaxitoxin, decarbamoyl-neosaxitoxin, saxitoxin, decarbamoyl-saxitoxin, domoic acid, 13-desmethyl spirolide C (SPX1), palytoxin and okadaic acid. Extraction and clean-up were carried out with a combination of Bond Elut LRC-C18 and Carbograph4 cartridges connected in series. Analyte separation was performed in gradient elution mode in 12 min with a Gemini C18 column. Compound detection was carried out in multiple reaction monitoring and in positive ionization mode for paralytic shellfish poisoning toxins, domoic acid, SPX1 and palytoxin, and in negative ionization mode for okadaic acid. The toxins were quantified with matrix-matched calibration curves constructed by spiked seawater samples (concentration levels 0.02–2 μg L−1 depending on the compound). The method was reproducible with intra-day and inter-day relative standard deviations ranging from 4 to 9{\%} and from 8 to 16{\%}, respectively. Good recoveries (84–105{\%}) and good accuracy (2–20{\%}) were obtained by spiking experiments. Limits of detection were calculated for each toxin and varied from 0.011 to 0.12 μg L−1 depending on the compound. The developed method was applied to cultured Ostreopsis cf. ovata samples. The proposed procedure may be considered a valuable alternative to existing methods for monitoring toxic microalgae, since it offers a rapid screening of target toxins, reduced organic solvent consumption, and handling of smaller sample volumes while providing good sensitivity and accuracy. Graphical Abstract: [Figure not available: see fulltext.].",
keywords = "Algal toxins, Column liquid chromatography, Harmful algal blooms, Seawater samples, Solid-phase extraction",
author = "Carmela Riccardi and Francesca Buiarelli and {Di Filippo}, Patrizia and Sisto Distratis and Luigi Giannetti and Maura Manganelli and Bruno Neri and Donatella Pomata and Mara Stefanelli",
year = "2018",
month = "2",
day = "1",
doi = "10.1007/s10337-017-3440-x",
language = "English",
volume = "81",
pages = "277--288",
journal = "Chromatographia",
issn = "0009-5893",
publisher = "Springer Vieweg",
number = "2",

}

TY - JOUR

T1 - Liquid Chromatography–Tandem Mass Spectrometry Method for the Screening of Eight Paralytic Shellfish Poisoning Toxins, Domoic Acid, 13-Desmethyl Spirolide C, Palytoxin and Okadaic Acid in Seawater

AU - Riccardi, Carmela

AU - Buiarelli, Francesca

AU - Di Filippo, Patrizia

AU - Distratis, Sisto

AU - Giannetti, Luigi

AU - Manganelli, Maura

AU - Neri, Bruno

AU - Pomata, Donatella

AU - Stefanelli, Mara

PY - 2018/2/1

Y1 - 2018/2/1

N2 - Abstract: A quick and reproducible screening analytical method for the simultaneous determination of algal toxins, belonging to different chemical classes, was developed to provide a toxin profile in seawater, useful to assess potential risks to environment and human health. The target compounds were: gonyautoxin-1,4, gonyautoxin-2,3, decarbamoylgonyautoxin-2,3, N‐sulfocarbamoyl-gonyautoxin-1,2, neosaxitoxin, decarbamoyl-neosaxitoxin, saxitoxin, decarbamoyl-saxitoxin, domoic acid, 13-desmethyl spirolide C (SPX1), palytoxin and okadaic acid. Extraction and clean-up were carried out with a combination of Bond Elut LRC-C18 and Carbograph4 cartridges connected in series. Analyte separation was performed in gradient elution mode in 12 min with a Gemini C18 column. Compound detection was carried out in multiple reaction monitoring and in positive ionization mode for paralytic shellfish poisoning toxins, domoic acid, SPX1 and palytoxin, and in negative ionization mode for okadaic acid. The toxins were quantified with matrix-matched calibration curves constructed by spiked seawater samples (concentration levels 0.02–2 μg L−1 depending on the compound). The method was reproducible with intra-day and inter-day relative standard deviations ranging from 4 to 9% and from 8 to 16%, respectively. Good recoveries (84–105%) and good accuracy (2–20%) were obtained by spiking experiments. Limits of detection were calculated for each toxin and varied from 0.011 to 0.12 μg L−1 depending on the compound. The developed method was applied to cultured Ostreopsis cf. ovata samples. The proposed procedure may be considered a valuable alternative to existing methods for monitoring toxic microalgae, since it offers a rapid screening of target toxins, reduced organic solvent consumption, and handling of smaller sample volumes while providing good sensitivity and accuracy. Graphical Abstract: [Figure not available: see fulltext.].

AB - Abstract: A quick and reproducible screening analytical method for the simultaneous determination of algal toxins, belonging to different chemical classes, was developed to provide a toxin profile in seawater, useful to assess potential risks to environment and human health. The target compounds were: gonyautoxin-1,4, gonyautoxin-2,3, decarbamoylgonyautoxin-2,3, N‐sulfocarbamoyl-gonyautoxin-1,2, neosaxitoxin, decarbamoyl-neosaxitoxin, saxitoxin, decarbamoyl-saxitoxin, domoic acid, 13-desmethyl spirolide C (SPX1), palytoxin and okadaic acid. Extraction and clean-up were carried out with a combination of Bond Elut LRC-C18 and Carbograph4 cartridges connected in series. Analyte separation was performed in gradient elution mode in 12 min with a Gemini C18 column. Compound detection was carried out in multiple reaction monitoring and in positive ionization mode for paralytic shellfish poisoning toxins, domoic acid, SPX1 and palytoxin, and in negative ionization mode for okadaic acid. The toxins were quantified with matrix-matched calibration curves constructed by spiked seawater samples (concentration levels 0.02–2 μg L−1 depending on the compound). The method was reproducible with intra-day and inter-day relative standard deviations ranging from 4 to 9% and from 8 to 16%, respectively. Good recoveries (84–105%) and good accuracy (2–20%) were obtained by spiking experiments. Limits of detection were calculated for each toxin and varied from 0.011 to 0.12 μg L−1 depending on the compound. The developed method was applied to cultured Ostreopsis cf. ovata samples. The proposed procedure may be considered a valuable alternative to existing methods for monitoring toxic microalgae, since it offers a rapid screening of target toxins, reduced organic solvent consumption, and handling of smaller sample volumes while providing good sensitivity and accuracy. Graphical Abstract: [Figure not available: see fulltext.].

KW - Algal toxins

KW - Column liquid chromatography

KW - Harmful algal blooms

KW - Seawater samples

KW - Solid-phase extraction

UR - http://www.scopus.com/inward/record.url?scp=85035092926&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=85035092926&partnerID=8YFLogxK

U2 - 10.1007/s10337-017-3440-x

DO - 10.1007/s10337-017-3440-x

M3 - Article

AN - SCOPUS:85035092926

VL - 81

SP - 277

EP - 288

JO - Chromatographia

JF - Chromatographia

SN - 0009-5893

IS - 2

ER -