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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
- Source :
- Chromatographia. 81:277-288
- Publication Year :
- 2017
- Publisher :
- Springer Science and Business Media LLC, 2017.
-
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.
- Subjects :
- Clinical Biochemistry
Neosaxitoxin
010501 environmental sciences
01 natural sciences
Biochemistry
Analytical Chemistry
chemistry.chemical_compound
Liquid chromatography–mass spectrometry
Palytoxin
seawater samples
algal toxins
column liquid chromatography
harmful algal blooms
solid-phase extraction
medicine
Paralytic shellfish poisoning
0105 earth and related environmental sciences
Saxitoxin
Chromatography
010401 analytical chemistry
Organic Chemistry
Selected reaction monitoring
Domoic acid
Okadaic acid
medicine.disease
0104 chemical sciences
chemistry
Subjects
Details
- ISSN :
- 16121112 and 00095893
- Volume :
- 81
- Database :
- OpenAIRE
- Journal :
- Chromatographia
- Accession number :
- edsair.doi.dedup.....67721df5e49c1f56db7a43fbad10be8f