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Sample preparation and liquid chromatography-tandem mass spectrometry for the analysis of selected Pacific ciguatoxins in blood samples.
J Chromatogr A. 2020 Jun 21; 1621:461050.JC

Abstract

Consumption of ciguatoxin-contaminated seafood can lead to ciguatera poisoning (CP). The diagnosis of CP in humans is based on the clinical symptoms after eating the fish from tropical or subtropical areas because no confirmatory clinical tests are available. One of the challenges for ciguatoxin analysis is their extremely low but toxicologically relevant concentration in biological samples. We previously reported a method using acetonitrile to precipitate proteins and extract the ciguatoxins simultaneously in whole blood samples from animals for toxin quantification by N2A cell-based assay. However, a test method for unambiguous confirmation of exposure of marine animals or humans to ciguatoxins is still needed. In the present study, we adopted the acetonitrile extraction method and added sample clean-up in the sample preparation for the determination of Pacific ciguatoxins CTX1B (aka P-CTX-1), 52-epi-54-deoxyCTX1B (aka P-CTX-2), and CTX3C (aka P-CTX-3C) in blood plasma by LC-MS/MS. We investigated sample clean-up, LC mobile phases, LC solvent programming, and settings of the two mass spectrometers (4000 Q TRAP and AB SCIEX Triple Quad 5500) in order to improve the ability to detect the Pacific ciguatoxins at ppt level. Rat blood plasma was used for the method development. Average recoveries of the three toxins in the rat plasma samples ranged from 90% to 116% with relative standard deviations of less than 15%. The method detection limits were still not low enough for the determination of the Pacific ciguatoxins in individual blood samples from Hawaiian monk seals with the two LC-MS systems. The methods were applied to a pooled sample of blood plasma collected from Hawaiian monk seals for confirmation of toxin exposure. This study will benefit monitoring of Pacific ciguatoxins in marine mammals and potentially humans by LC-MS/MS.

Authors+Show Affiliations

CSS, Inc. under contract to NOAA, HAB Monitoring & Reference Branch, Stressor Detection and Impacts Division, National Centers for Coastal Ocean Science, NOAA National Ocean Service, 219 Fort Johnson Road, Charleston, SC 29412, USA.CSS, Inc. under contract to NOAA, HAB Monitoring & Reference Branch, Stressor Detection and Impacts Division, National Centers for Coastal Ocean Science, NOAA National Ocean Service, 219 Fort Johnson Road, Charleston, SC 29412, USA.HAB Monitoring & Reference Branch, Stressor Detection and Impacts Division, National Centers for Coastal Ocean Science, NOAA National Ocean Service, 219 Fort Johnson Road, Charleston, SC 29412, USA.Pacific Islands Fisheries Science Center, National Marine Fisheries Service, NOAA, 1845 Wasp Boulevard, No. 176, Honolulu, HI 96818, USA.HAB Monitoring & Reference Branch, Stressor Detection and Impacts Division, National Centers for Coastal Ocean Science, NOAA National Ocean Service, 219 Fort Johnson Road, Charleston, SC 29412, USA. Electronic address: john.ramsdell@noaa.gov.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

32265050

Citation

Wang, Zhihong, et al. "Sample Preparation and Liquid Chromatography-tandem Mass Spectrometry for the Analysis of Selected Pacific Ciguatoxins in Blood Samples." Journal of Chromatography. A, vol. 1621, 2020, p. 461050.
Wang Z, Fuquay JM, Ledreux A, et al. Sample preparation and liquid chromatography-tandem mass spectrometry for the analysis of selected Pacific ciguatoxins in blood samples. J Chromatogr A. 2020;1621:461050.
Wang, Z., Fuquay, J. M., Ledreux, A., Barbieri, M., & Ramsdell, J. S. (2020). Sample preparation and liquid chromatography-tandem mass spectrometry for the analysis of selected Pacific ciguatoxins in blood samples. Journal of Chromatography. A, 1621, 461050. https://doi.org/10.1016/j.chroma.2020.461050
Wang Z, et al. Sample Preparation and Liquid Chromatography-tandem Mass Spectrometry for the Analysis of Selected Pacific Ciguatoxins in Blood Samples. J Chromatogr A. 2020 Jun 21;1621:461050. PubMed PMID: 32265050.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Sample preparation and liquid chromatography-tandem mass spectrometry for the analysis of selected Pacific ciguatoxins in blood samples. AU - Wang,Zhihong, AU - Fuquay,Jennifer Maucher, AU - Ledreux,Aurelie, AU - Barbieri,Michelle, AU - Ramsdell,John S, Y1 - 2020/03/16/ PY - 2020/01/23/received PY - 2020/03/13/revised PY - 2020/03/14/accepted PY - 2020/4/9/pubmed PY - 2020/7/24/medline PY - 2020/4/9/entrez KW - Blood KW - Ciguatera KW - Hawaiian monk seal KW - LC–MS KW - Pacific ciguatoxins SP - 461050 EP - 461050 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1621 N2 - Consumption of ciguatoxin-contaminated seafood can lead to ciguatera poisoning (CP). The diagnosis of CP in humans is based on the clinical symptoms after eating the fish from tropical or subtropical areas because no confirmatory clinical tests are available. One of the challenges for ciguatoxin analysis is their extremely low but toxicologically relevant concentration in biological samples. We previously reported a method using acetonitrile to precipitate proteins and extract the ciguatoxins simultaneously in whole blood samples from animals for toxin quantification by N2A cell-based assay. However, a test method for unambiguous confirmation of exposure of marine animals or humans to ciguatoxins is still needed. In the present study, we adopted the acetonitrile extraction method and added sample clean-up in the sample preparation for the determination of Pacific ciguatoxins CTX1B (aka P-CTX-1), 52-epi-54-deoxyCTX1B (aka P-CTX-2), and CTX3C (aka P-CTX-3C) in blood plasma by LC-MS/MS. We investigated sample clean-up, LC mobile phases, LC solvent programming, and settings of the two mass spectrometers (4000 Q TRAP and AB SCIEX Triple Quad 5500) in order to improve the ability to detect the Pacific ciguatoxins at ppt level. Rat blood plasma was used for the method development. Average recoveries of the three toxins in the rat plasma samples ranged from 90% to 116% with relative standard deviations of less than 15%. The method detection limits were still not low enough for the determination of the Pacific ciguatoxins in individual blood samples from Hawaiian monk seals with the two LC-MS systems. The methods were applied to a pooled sample of blood plasma collected from Hawaiian monk seals for confirmation of toxin exposure. This study will benefit monitoring of Pacific ciguatoxins in marine mammals and potentially humans by LC-MS/MS. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/32265050/Sample_preparation_and_liquid_chromatography_tandem_mass_spectrometry_for_the_analysis_of_selected_Pacific_ciguatoxins_in_blood_samples_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(20)30262-4 DB - PRIME DP - Unbound Medicine ER -