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An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3.
Toxicon. 2015 Dec 15; 108:249-56.T

Abstract

Ciguatera fish poisoning is a debilitating human neuro-intoxication caused by consumption of tropical marine organisms, contaminated with bioaccumulated ciguatoxins (CTXs). The growing number of cases coupled with the high toxicity of CTXs makes their reliable detection and quantification of paramount importance. Three commonly occurring ciguatoxins, P-CTX-1, 2 and 3 from five different ciguatoxic Spanish mackerel (Scomberomorus commerson), were used to assess the effectiveness of different extraction techniques: homogenization (high powered blending vs. ultrasonication); C-18 column sizes (500 mg vs. 900 mg); and a novel HILIC SPE cleanup. Despite minor differences, blending and sonication proved equally effective. Larger 900 mg columns offered a greater extraction efficiency, increasing detected P-CTX-1 by 37% (P < 0.001). The newly adapted cleanup was highly effective at reducing co-eluting phospholipids thereby reducing matrix effects and increasing detectable CTXs by HPLC-MS/MS. Silica cleanup extraction efficiencies were also compared between the highly effective and validated ciguatoxin rapid extraction method (CREM) and current best practice extraction method employed by Queensland Health (QH). Overall, the QH protocol proved more effective, especially when paired with the newly adapted cleanup, as this increased the amount of extracted P-CTX-1 by 46% (P < 0.01), P-CTX-2 by 10% and P-CTX-3 by 71% (P = 0.001). This study suggests the QH protocol utilizing a 900 mg C-18 column and newly adapted HILIC SPE cleanup was most effective at extracting P-CTX-1, -2, -3. Specifically P-CTX-1, the primary ciguatoxin congener of concern due to its extremely high potency and an ability to cause CFP at 0.1 μg/kg following consumption of carnivorous fish flesh. Despite being more time intensive (an additional 85 min per batch of 12 samples), this will be especially effective for assessing lower toxin burdens, which may be near the limit of detection.

Authors+Show Affiliations

James Cook University, Centre for Sustainable Tropical Fisheries and Aquaculture, James Cook University, James Cook Drive, Townsville, QLD 4811, Australia. Electronic address: Lauren.meyer@my.jcu.edu.au.Queensland Health Forensic and Scientific Services, 39 Kessels Road, Coopers Plains, QLD 4108, Australia.James Cook University, Centre for Sustainable Tropical Fisheries and Aquaculture, James Cook University, James Cook Drive, Townsville, QLD 4811, Australia.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

26541571

Citation

Meyer, Lauren, et al. "An Updated Ciguatoxin Extraction Method and Silica Cleanup for Use With HPLC-MS/MS for the Analysis of P-CTX-1, PCTX-2 and P-CTX-3." Toxicon : Official Journal of the International Society On Toxinology, vol. 108, 2015, pp. 249-56.
Meyer L, Carter S, Capper A. An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3. Toxicon. 2015;108:249-56.
Meyer, L., Carter, S., & Capper, A. (2015). An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3. Toxicon : Official Journal of the International Society On Toxinology, 108, 249-56. https://doi.org/10.1016/j.toxicon.2015.10.021
Meyer L, Carter S, Capper A. An Updated Ciguatoxin Extraction Method and Silica Cleanup for Use With HPLC-MS/MS for the Analysis of P-CTX-1, PCTX-2 and P-CTX-3. Toxicon. 2015 Dec 15;108:249-56. PubMed PMID: 26541571.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3. AU - Meyer,Lauren, AU - Carter,Steve, AU - Capper,Angela, Y1 - 2015/11/02/ PY - 2015/09/04/received PY - 2015/10/24/revised PY - 2015/10/28/accepted PY - 2015/11/7/entrez PY - 2015/11/7/pubmed PY - 2016/10/13/medline KW - Ciguatera KW - Ciguatoxin KW - Extraction efficiency KW - HPLC-MS/MS SP - 249 EP - 56 JF - Toxicon : official journal of the International Society on Toxinology JO - Toxicon VL - 108 N2 - Ciguatera fish poisoning is a debilitating human neuro-intoxication caused by consumption of tropical marine organisms, contaminated with bioaccumulated ciguatoxins (CTXs). The growing number of cases coupled with the high toxicity of CTXs makes their reliable detection and quantification of paramount importance. Three commonly occurring ciguatoxins, P-CTX-1, 2 and 3 from five different ciguatoxic Spanish mackerel (Scomberomorus commerson), were used to assess the effectiveness of different extraction techniques: homogenization (high powered blending vs. ultrasonication); C-18 column sizes (500 mg vs. 900 mg); and a novel HILIC SPE cleanup. Despite minor differences, blending and sonication proved equally effective. Larger 900 mg columns offered a greater extraction efficiency, increasing detected P-CTX-1 by 37% (P < 0.001). The newly adapted cleanup was highly effective at reducing co-eluting phospholipids thereby reducing matrix effects and increasing detectable CTXs by HPLC-MS/MS. Silica cleanup extraction efficiencies were also compared between the highly effective and validated ciguatoxin rapid extraction method (CREM) and current best practice extraction method employed by Queensland Health (QH). Overall, the QH protocol proved more effective, especially when paired with the newly adapted cleanup, as this increased the amount of extracted P-CTX-1 by 46% (P < 0.01), P-CTX-2 by 10% and P-CTX-3 by 71% (P = 0.001). This study suggests the QH protocol utilizing a 900 mg C-18 column and newly adapted HILIC SPE cleanup was most effective at extracting P-CTX-1, -2, -3. Specifically P-CTX-1, the primary ciguatoxin congener of concern due to its extremely high potency and an ability to cause CFP at 0.1 μg/kg following consumption of carnivorous fish flesh. Despite being more time intensive (an additional 85 min per batch of 12 samples), this will be especially effective for assessing lower toxin burdens, which may be near the limit of detection. SN - 1879-3150 UR - https://www.unboundmedicine.com/medline/citation/26541571/An_updated_ciguatoxin_extraction_method_and_silica_cleanup_for_use_with_HPLC_MS/MS_for_the_analysis_of_P_CTX_1_PCTX_2_and_P_CTX_3_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0041-0101(15)30124-0 DB - PRIME DP - Unbound Medicine ER -