{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,1,15]],"date-time":"2026-01-15T04:30:58Z","timestamp":1768451458006,"version":"3.49.0"},"reference-count":28,"publisher":"Oxford University Press (OUP)","issue":"5","license":[{"start":{"date-parts":[[2021,4,8]],"date-time":"2021-04-08T00:00:00Z","timestamp":1617840000000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/creativecommons.org\/licenses\/by-nc-nd\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":[],"published-print":{"date-parts":[[2021,9,27]]},"abstract":"<jats:title>Abstract<\/jats:title>\n               <jats:sec>\n                  <jats:title>Background<\/jats:title>\n                  <jats:p>Ciguatera fish poisoning (CFP) poses a serious threat to both public health and the use of aquatic resources from the various warm-water regions of the world. Hence, a process for the efficient determination of the relevant toxins is required.<\/jats:p>\n               <\/jats:sec>\n               <jats:sec>\n                  <jats:title>Objective<\/jats:title>\n                  <jats:p>We sought to develop and validate the first LC-MS\/MS method to quantify the major toxins prevalent in fish from the Pacific Ocean.<\/jats:p>\n               <\/jats:sec>\n               <jats:sec>\n                  <jats:title>Method<\/jats:title>\n                  <jats:p>Toxins were extracted from fish flesh (2\u2009g) using a methanol\u2013water mixture (9:1, v\/v). The extract was heated at 80\u00b0C, and low-polarity lipids were eliminated using hexane, initially from the basic solution and later from the acidic solution. The cleanup was performed using solid-phase extraction, Florisil, silica, reversed-phase C18, and primary secondary amine columns. A validation study was conducted by spiking fish flesh with two representative toxins having different skeletal structures and polarities and was calibrated by NMR (qNMR) spectroscopy.<\/jats:p>\n               <\/jats:sec>\n               <jats:sec>\n                  <jats:title>Results<\/jats:title>\n                  <jats:p>The validation parameters for the ciguatera toxins CTX1B and CTX3C at spiked levels of 0.1\u2009\u00b5g\/kg were as follows: repeatabilities of 2.3\u20133.5% and 3.2\u20135.3%; intermediate precisions of 6.3\u20139.8% and 6.0\u20137.4%; recoveries of 80\u2013107% and 95\u2013120%, respectively. The lowest detection levels were 0.004\u2009\u00b5g\/kg for CTX1B, 0.005\u2009\u00b5g\/kg for 51-hydroxyCTX3C, and 0.009\u2009\u00b5g\/kg for CTX3C.<\/jats:p>\n               <\/jats:sec>\n               <jats:sec>\n                  <jats:title>Conclusions<\/jats:title>\n                  <jats:p>The described method practically clears the international action level of 0.01\u2009\u00b5g\/kg CTX1B equivalents set by the U.S. Food and Drug Administration and the European Food Safety Authority and satisfies the global standards set by Codex and AOAC INTERNATIONAL.<\/jats:p>\n               <\/jats:sec>\n               <jats:sec>\n                  <jats:title>Highlights<\/jats:title>\n                  <jats:p>A validation study for an LC-MS\/MS method for ciguatoxin detection was completed for the first time using calibrated toxin standards.<\/jats:p>\n               <\/jats:sec>","DOI":"10.1093\/jaoacint\/qsab052","type":"journal-article","created":{"date-parts":[[2021,4,7]],"date-time":"2021-04-07T19:13:45Z","timestamp":1617822825000},"page":"1272-1281","source":"Crossref","is-referenced-by-count":19,"title":["Development and Validation of an LC-MS\/MS Method for the Ultra-Trace Analysis of Pacific Ciguatoxins in Fish"],"prefix":"10.1093","volume":"104","author":[{"given":"Mika","family":"Nagae","sequence":"first","affiliation":[{"name":"Japan Food Research Laboratories, Tama Laboratory, 6-11-10 Nagayama, Tama, Tokyo 206-0025, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6045-0455","authenticated-orcid":false,"given":"Tomoji","family":"Igarashi","sequence":"additional","affiliation":[{"name":"Japan Food Research Laboratories, Tama Laboratory, 6-11-10 Nagayama, Tama, Tokyo 206-0025, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Kazushi","family":"Mizukoshi","sequence":"additional","affiliation":[{"name":"Japan Food Research Laboratories, Tama Laboratory, 6-11-10 Nagayama, Tama, Tokyo 206-0025, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Kyoko","family":"Kuniyoshi","sequence":"additional","affiliation":[{"name":"National Institute of Health Sciences, 3-25-26 Tonomachi, Kawasaki, Kanagawa 210-9501, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1130-4491","authenticated-orcid":false,"given":"Naomasa","family":"Oshiro","sequence":"additional","affiliation":[{"name":"National Institute of Health Sciences, 3-25-26 Tonomachi, Kawasaki, Kanagawa 210-9501, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Takeshi","family":"Yasumoto","sequence":"additional","affiliation":[{"name":"Japan Food Research Laboratories, Tama Laboratory, 6-11-10 Nagayama, Tama, Tokyo 206-0025, Japan"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"286","published-online":{"date-parts":[[2021,4,8]]},"reference":[{"key":"2021092712421548800_qsab052-B1","doi-asserted-by":"crossref","first-page":"228","DOI":"10.1002\/tcr.1010","volume":"1","author":"Yasumoto","year":"2001","journal-title":"Chem. 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