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Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy.
Mar Drugs. 2017 Oct 12; 15(10)MD

Abstract

The absolute quantification of five toxins involved in ciguatera fish poisoning (CFP) in the Pacific was carried out by quantitative ¹H-NMR. The targeted toxins were ciguatoxin-1B (CTX1B), 52-epi-54-deoxyciguatoxin-1B (epideoxyCTX1B), ciguatoxin-3C (CTX3C), 51-hydroxyciguatoxin-3C (51OHCTX3C), and ciguatoxin-4A (CTX4A). We first calibrated the residual protons of pyridine-d₅ using certified reference material, 1,4-BTMSB-d₄, prepared the toxin solutions with the calibrated pyridin-d₅, measured the ¹H-NMR spectra, and quantified the toxin using the calibrated residual protons as the internal standard. The absolute quantification was carried out by comparing the signal intensities between the selected protons of the target toxin and the residual protons of the calibrated pyridine-d₅. The proton signals residing on the ciguatoxins (CTXs) to be used for quantification were carefully selected for those that were well separated from adjacent signals including impurities and that exhibited an effective intensity. To quantify CTX1B and its congeners, the olefin protons in the side chain were judged appropriate for use. The quantification was achievable with nano-molar solutions. The probable errors for uncertainty, calculated on respective toxins, ranged between 3% and 16%. The contamination of the precious toxins with nonvolatile internal standards was thus avoided. After the evaporation of pyridine-d₅, the calibrated CTXs were ready for use as the reference standard in the quantitative analysis of ciguatoxins by LC/MS.

Authors+Show Affiliations

Japan Food Research Laboratories, Tama Laboratory, Nagayama 6-11-10, Tama, Tokyo 206-0025, Japan. katout@jfrl.or.jp.Japan Food Research Laboratories, Tama Laboratory, Nagayama 6-11-10, Tama, Tokyo 206-0025, Japan. yasumotot@jfrl.or.jp.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

29023382

Citation

Kato, Tsuyoshi, and Takeshi Yasumoto. "Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy." Marine Drugs, vol. 15, no. 10, 2017.
Kato T, Yasumoto T. Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy. Mar Drugs. 2017;15(10).
Kato, T., & Yasumoto, T. (2017). Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy. Marine Drugs, 15(10). https://doi.org/10.3390/md15100309
Kato T, Yasumoto T. Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy. Mar Drugs. 2017 Oct 12;15(10) PubMed PMID: 29023382.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy. AU - Kato,Tsuyoshi, AU - Yasumoto,Takeshi, Y1 - 2017/10/12/ PY - 2017/09/08/received PY - 2017/09/29/revised PY - 2017/10/09/accepted PY - 2017/10/13/entrez PY - 2017/10/13/pubmed PY - 2018/6/2/medline KW - ciguatoxin-1B KW - ciguatoxin-3C KW - qNMR JF - Marine drugs JO - Mar Drugs VL - 15 IS - 10 N2 - The absolute quantification of five toxins involved in ciguatera fish poisoning (CFP) in the Pacific was carried out by quantitative ¹H-NMR. The targeted toxins were ciguatoxin-1B (CTX1B), 52-epi-54-deoxyciguatoxin-1B (epideoxyCTX1B), ciguatoxin-3C (CTX3C), 51-hydroxyciguatoxin-3C (51OHCTX3C), and ciguatoxin-4A (CTX4A). We first calibrated the residual protons of pyridine-d₅ using certified reference material, 1,4-BTMSB-d₄, prepared the toxin solutions with the calibrated pyridin-d₅, measured the ¹H-NMR spectra, and quantified the toxin using the calibrated residual protons as the internal standard. The absolute quantification was carried out by comparing the signal intensities between the selected protons of the target toxin and the residual protons of the calibrated pyridine-d₅. The proton signals residing on the ciguatoxins (CTXs) to be used for quantification were carefully selected for those that were well separated from adjacent signals including impurities and that exhibited an effective intensity. To quantify CTX1B and its congeners, the olefin protons in the side chain were judged appropriate for use. The quantification was achievable with nano-molar solutions. The probable errors for uncertainty, calculated on respective toxins, ranged between 3% and 16%. The contamination of the precious toxins with nonvolatile internal standards was thus avoided. After the evaporation of pyridine-d₅, the calibrated CTXs were ready for use as the reference standard in the quantitative analysis of ciguatoxins by LC/MS. SN - 1660-3397 UR - https://www.unboundmedicine.com/medline/citation/29023382/Quantification_of_Representative_Ciguatoxins_in_the_Pacific_Using_Quantitative_Nuclear_Magnetic_Resonance_Spectroscopy_ L2 - https://www.mdpi.com/resolver?pii=md15100309 DB - PRIME DP - Unbound Medicine ER -