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1

Boundy, Michael J., D. Tim Harwood, Andreas Kiermeier, Cath McLeod, Jeane Nicolas, and Sarah Finch. "Risk Assessment of Pectenotoxins in New Zealand Bivalve Molluscan Shellfish, 2009–2019." Toxins 12, no. 12 (December 6, 2020): 776. http://dx.doi.org/10.3390/toxins12120776.

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Pectenotoxins (PTXs) are produced by Dinophysis spp., along with okadaic acid, dinophysistoxin 1, and dinophysistoxin 2. The okadaic acid group toxins cause diarrhetic shellfish poisoning (DSP), so are therefore regulated. New Zealand currently includes pectenotoxins within the DSP regulations. To determine the impact of this decision, shellfish biotoxin data collected between 2009 and 2019 were examined. They showed that 85 samples exceeded the DSP regulatory limit (0.45%) and that excluding pectenotoxins would have reduced this by 10% to 76 samples. The incidence (1.3%) and maximum concentrations of pectenotoxins (0.079 mg/kg) were also found to be low, well below the current European Food Safety Authority (EFSA) safe limit of 0.12 mg/kg. Inclusion within the DSP regulations is scientifically flawed, as pectenotoxins and okadaic acid have a different mechanism of action, meaning that their toxicities are not additive, which is the fundamental principle of grouping toxins. Furthermore, evaluation of the available toxicity data suggests that pectenotoxins have very low oral toxicity, with recent studies showing no oral toxicity in mice dosed with the PTX analogue PTX2 at 5000 µg/kg. No known human illnesses have been reported due to exposure to pectenotoxins in shellfish, a fact which combined with the toxicity data indicates that they pose negligible risk to humans. Regulatory policies should be commensurate with the level of risk, thus deregulation of PTXs ought to be considered, a stance already adopted by some countries.
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2

Krock, Bernd, Urban Tillmann, Andrew I. Selwood, and Allan D. Cembella. "Unambiguous identification of pectenotoxin-1 and distribution of pectenotoxins in plankton from the North Sea." Toxicon 52, no. 8 (December 2008): 927–35. http://dx.doi.org/10.1016/j.toxicon.2008.09.006.

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3

Reguera, Beatriz, and Juan Blanco. "Dinophysis Toxins: Distribution, Fate in Shellfish and Impacts." Toxins 11, no. 7 (July 16, 2019): 413. http://dx.doi.org/10.3390/toxins11070413.

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Several planktonic dinoflagellate species of the genus Dinophysis produce one or two groups of lipophilic toxins: (i) okadaic acid (OA) and its derivatives, the dinophysistoxins (DTXs), and (ii) pectenotoxins (PTXs) [...]
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4

Burgess, Vanessa, and Glen Shaw. "Pectenotoxins — an issue for public health." Environment International 27, no. 4 (October 2001): 275–83. http://dx.doi.org/10.1016/s0160-4120(01)00058-7.

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5

Sasaki, Katsunori, Jeffrey L. C. Wright, and Takeshi Yasumoto. "Identification and Characterization of Pectenotoxin (PTX) 4 and PTX7 as Spiroketal Stereoisomers of Two Previously Reported Pectenotoxins." Journal of Organic Chemistry 63, no. 8 (April 1998): 2475–80. http://dx.doi.org/10.1021/jo971310b.

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6

Espiña, B., M. C. Louzao, I. R. Ares, E. Cagide, M. R. Vieytes, F. V. Vega, J. A. Rubiolo, et al. "Cytoskeletal toxicity of pectenotoxins in hepatic cells." British Journal of Pharmacology 155, no. 6 (November 2008): 934–44. http://dx.doi.org/10.1038/bjp.2008.323.

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7

Halim, Rosliana, and Margaret A. Brimble. "Synthetic studies towards the pectenotoxins: a review." Organic & Biomolecular Chemistry 4, no. 22 (2006): 4048. http://dx.doi.org/10.1039/b611531b.

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8

SASAKI, K., J. L. C. WRIGHT, and T. YASUMOTO. "ChemInform Abstract: Identification and Characterization of Pectenotoxin (PTX) 4 and PTX7 as Spiroketal Stereoisomers of Two Previously Reported Pectenotoxins." ChemInform 29, no. 33 (June 20, 2010): no. http://dx.doi.org/10.1002/chin.199833297.

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9

Halim, Rosliana, Margaret A. Brimble, and Jörn Merten. "Synthesis of the ABC Fragment of the Pectenotoxins." Organic Letters 7, no. 13 (June 2005): 2659–62. http://dx.doi.org/10.1021/ol0507975.

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10

Brimble, Margaret, Amanda Heapy, and Thomas Wagner. "Synthesis of the FG Fragment of the Pectenotoxins." Synlett 2007, no. 15 (September 2007): 2359–62. http://dx.doi.org/10.1055/s-2007-985600.

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11

Brimble, Margaret, Amanda Heapy, and Thomas Wagner. "Synthesis of the FG Fragment of the Pectenotoxins." Synlett 2008, no. 11 (June 20, 2008): 1746. http://dx.doi.org/10.1055/s-2008-1067135.

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12

Brimble, Margaret A., and Rosliana Halim. "Synthetic studies toward shellfish toxins containing spiroacetal units." Pure and Applied Chemistry 79, no. 2 (January 1, 2007): 153–62. http://dx.doi.org/10.1351/pac200779020153.

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The synthesis of the ABC spiroacetal-containing fragment of the marine biotoxins, the pectenotoxins (PTXs), is described. The synthetic strategy involves appendage of the highly substituted tetrahydofuran C ring to the AB spiroacetal unit via stereocontrolled cyclization of a γ-hydroxyepoxide. The bis-spiroacetal moiety of the spirolide family of shellfish toxins is also described, making use of an iterative radical oxidative cyclization strategy.
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13

Dzhembekova, Nina, Snejana Moncheva, Nataliya Slabakova, Ivelina Zlateva, Satoshi Nagai, Stephan Wietkamp, Marvin Wellkamp, Urban Tillmann, and Bernd Krock. "New Knowledge on Distribution and Abundance of Toxic Microalgal Species and Related Toxins in the Northwestern Black Sea." Toxins 14, no. 10 (October 6, 2022): 685. http://dx.doi.org/10.3390/toxins14100685.

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Numerous potentially toxic plankton species commonly occur in the Black Sea, and phycotoxins have been reported. However, the taxonomy, phycotoxin profiles, and distribution of harmful microalgae in the basin are still understudied. An integrated microscopic (light microscopy) and molecular (18S rRNA gene metabarcoding and qPCR) approach complemented with toxin analysis was applied at 41 stations in the northwestern part of the Black Sea for better taxonomic coverage and toxin profiling in natural populations. The combined dataset included 20 potentially toxic species, some of which (Dinophysis acuminata, Dinophysis acuta, Gonyaulax spinifera, and Karlodinium veneficum) were detected in over 95% of the stations. In parallel, pectenotoxins (PTX-2 as a major toxin) were registered in all samples, and yessotoxins were present at most of the sampling points. PTX-1 and PTX-13, as well as some YTX variants, were recorded for the first time in the basin. A positive correlation was found between the cell abundance of Dinophysis acuta and pectenotoxins, and between Lingulodinium polyedra and Protoceratium reticulatum and yessotoxins. Toxic microalgae and toxin variant abundance and spatial distribution was associated with environmental parameters. Despite the low levels of the identified phycotoxins and their low oral toxicity, chronic toxic exposure could represent an ecosystem and human health hazard.
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14

Fujiwara, Kenshu, Masanori Kobayashi, Fuyuki Yamamoto, Yu-ichi Aki, Mariko Kawamura, Daisuke Awakura, Seiji Amano, et al. "Synthesis of the common left-half part of pectenotoxins." Tetrahedron Letters 46, no. 30 (July 2005): 5067–69. http://dx.doi.org/10.1016/j.tetlet.2005.05.062.

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15

McCarron, Pearse, Elliott Wright, and Michael A. Quilliam. "Liquid Chromatography/Mass Spectrometry of Domoic Acid and Lipophilic Shellfish Toxins with Selected Reaction Monitoring and Optional Confirmation by Library Searching of Product Ion Spectra." Journal of AOAC INTERNATIONAL 97, no. 2 (March 1, 2014): 316–24. http://dx.doi.org/10.5740/jaoacint.sgemccarron.

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Abstract LC/MS methodology for the analysis of domoic acidand lipophilic toxins in shellfish was developed using a hybrid triple quadrupole linear ion trap mass spectrometer. For routine quantitation a scheduled selected reaction monitoring (SRM) method for the analysis of domoic acid, okadaic acid, dinophysistoxins,azaspiracids, pectenotoxins, yessotoxins, gymnodimines, spirolides, and pinnatoxins was developed and validated. The method performed well in terms of LOD, linearity, precision, and trueness. Taking advantageof the high instrument sensitivity, matrix effects were mitigated by reducing the amount of sample introduced to the mass spectrometer. Optionally, samples can be analyzed using information dependent acquisition (IDA) methods, either in positive or negative mode, which can provide an extra level of confirmationby matching the full product ion spectra acquired for a sample with those from a specially constructedspectral library. Methods were applied to the analysisof a new certified reference material and Canadian mussels (Mytilus edulis) implicated in a 2011 diarrhetic shellfish poisoning (DSP) incident. The scheduled SRM method enabled the screening and quantitation of multiple phycotoxins. As DSPhad not previously been observed in this area of Canada,positive identification of putative toxins was accomplished using the IDA and spectral search method. Analysis of the 2011 toxic mussel samples revealed thepresence of high levels of dinophysistoxin-1, which explained the DSP symptoms, as well as pectenotoxins, yessotoxins, and variety of cyclic imines.
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16

Amano, Seiji, Kenshu Fujiwara, and Akio Murai. "The Synthesis of the Common C31-C40 Fragment of Pectenotoxins." Synlett 1997, no. 11 (November 1997): 1300–1302. http://dx.doi.org/10.1055/s-1997-1033.

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17

Heapy, Amanda M., and Margaret A. Brimble. "Synthesis of the FG ring fragment of pectenotoxins 1–9." Tetrahedron 66, no. 29 (July 2010): 5424–31. http://dx.doi.org/10.1016/j.tet.2010.05.027.

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18

Doucet, Erin, Neil N. Ross, and Michael A. Quilliam. "Enzymatic hydrolysis of esterified diarrhetic shellfish poisoning toxins and pectenotoxins." Analytical and Bioanalytical Chemistry 389, no. 1 (July 28, 2007): 335–42. http://dx.doi.org/10.1007/s00216-007-1489-3.

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19

Allingham, John S., Christopher O. Miles, and Ivan Rayment. "A Structural Basis for Regulation of Actin Polymerization by Pectenotoxins." Journal of Molecular Biology 371, no. 4 (August 2007): 959–70. http://dx.doi.org/10.1016/j.jmb.2007.05.056.

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20

Zhaoxin, Li. "Accumulation and depuration of pectenotoxins in brown crab Cancer pagurus." Chinese Journal of Oceanology and Limnology 27, no. 2 (May 2009): 389–94. http://dx.doi.org/10.1007/s00343-009-9109-z.

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21

McNabb, Paul, Andrew I. Selwood, Patrick T. Holland, J. Aasen, T. Aune, G. Eaglesham, P. Hess, et al. "Multiresidue Method for Determination of Algal Toxins in Shellfish: Single-Laboratory Validation and Interlaboratory Study." Journal of AOAC INTERNATIONAL 88, no. 3 (May 1, 2005): 761–72. http://dx.doi.org/10.1093/jaoac/88.3.761.

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Abstract A method that uses liquid chromatography with tandem mass spectrometry (LC/MS/MS) has been developed for the highly sensitive and specific determination of amnesic shellfish poisoning toxins, diarrhetic shellfish poisoning toxins, and other lipophilic algal toxins and metabolites in shellfish. The method was subjected to a full single-laboratory validation and a limited interlaboratory study. Tissue homogenates are blended with methanol-water (9 + 1), and the centrifuged extract is cleaned up with a hexane wash. LC/MS/MS (triple quadrupole) is used for quantitative analysis with reversed-phase gradient elution (acidic buffer), electrospray ionization (positive and negative ion switching), and multiple-reaction monitoring. Ester forms of dinophysis toxins are detected as the parent toxins after hydrolysis of the methanolic extract. The method is quantitative for 6 key toxins when reference standards are available: azaspiracid-1 (AZA1), domoic acid (DA), gymnodimine (GYM), okadaic acid (OA), pectenotoxin-2 (PTX2), and yessotoxin (YTX). Relative response factors are used to estimate the concentrations of other toxins: azaspiracid-2 and -3 (AZA2 and AZA3), dinophysis toxin-1 and -2 (DTX1 and DTX2), other pectenotoxins (PTX1, PTX6, and PTX11), pectenotoxin secoacid metabolites (PTX2-SA and PTX11-SA) and their 7-epimers, spirolides, and homoYTX and YTX metabolites (45-OHYTX and carboxyYTX). Validation data have been gathered for Greenshell mussel, Pacific oyster, cockle, and scallop roe via fortification and natural contamination. For the 6 key toxins at fortification levels of 0.05–0.20 mg/kg, recoveries were 71–99% and single laboratory reproducibilities, relative standard deviations (RSDs), were 10–24%. Limits of detection were <0.02 mg/kg. Extractability data were also obtained for several toxins by using successive extractions of naturally contaminated mussel samples. A preliminary interlaboratory study was conducted with a set of toxin standards and 4 mussel extracts. The data sets from 8 laboratories for the 6 key toxins plus DTX1 and DTX2 gave within-laboratories repeatability (RSDr) of 8–12%, except for PTX-2. Between-laboratories reproducibility (RSDR) values were compared with the Horwitz criterion and ranged from good to adequate for 7 key toxins (HorRat values of 0.8–2.0).
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22

Espiña, Begoña, and Juan A. Rubiolo. "Marine toxins and the cytoskeleton: pectenotoxins, unusual macrolides that disrupt actin." FEBS Journal 275, no. 24 (October 29, 2008): 6082–88. http://dx.doi.org/10.1111/j.1742-4658.2008.06714.x.

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23

Vale, Paulo. "Differential dynamics of dinophysistoxins and pectenotoxins, part II: Offshore bivalve species." Toxicon 47, no. 2 (February 2006): 163–73. http://dx.doi.org/10.1016/j.toxicon.2005.10.009.

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24

Fabro, Elena, Gastón O. Almandoz, Martha E. Ferrario, Mónica S. Hoffmeyer, Rosa E. Pettigrosso, Román Uibrig, and Bernd Krock. "Co-occurrence of Dinophysis tripos and pectenotoxins in Argentinean shelf waters." Harmful Algae 42 (February 2015): 25–33. http://dx.doi.org/10.1016/j.hal.2014.12.005.

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25

Matsushima, Ryoji, Saori Kikutsugi, Ryuichi Watanabe, Hajime Uchida, Takeshi Yasumoto, Hiroshi Nagai, Masaki Kaneniwa, and Toshiyuki Suzuki. "Comparison of cytotoxicity among pectenotoxin-2 and other oxidized pectenotoxins in a rat myoblast cell line (L6) and a human rhabdomyosarcoma cell line (RD)." Fundamental Toxicological Sciences 2, no. 1 (2015): 49–54. http://dx.doi.org/10.2131/fts.2.49.

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26

Kouridaki, Antonia, Tamsyn Montagnon, Dimitris Kalaitzakis, and Georgios Vassilikogiannakis. "Using singlet oxygen to synthesise the CDE-ring system of the pectenotoxins." Org. Biomol. Chem. 11, no. 4 (2013): 537–41. http://dx.doi.org/10.1039/c2ob27158c.

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27

AMANO, S., K. FUJIWARA, and A. MURAI. "ChemInform Abstract: The Synthesis of the Common C31-C40 Fragment of Pectenotoxins." ChemInform 29, no. 9 (June 23, 2010): no. http://dx.doi.org/10.1002/chin.199809267.

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28

Suzuki, Toshiyuki, Veronica Beuzenberg, Lincoln Mackenzie, and Michael A. Quilliam. "Liquid chromatography–mass spectrometry of spiroketal stereoisomers of pectenotoxins and the analysis of novel pectenotoxin isomers in the toxic dinoflagellate Dinophysis acuta from New Zealand." Journal of Chromatography A 992, no. 1-2 (April 2003): 141–50. http://dx.doi.org/10.1016/s0021-9673(03)00324-8.

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29

Abouabdellaha, Rachid, Asmae Bennouna, Jaouad El Attar, Katrin Erler, Mina Dellal, Abdel ghani Chafik, and Abdelatif Moukrim. "Diarrhetic shellfish poisoning toxin profile of shellfish from Southern Atlantic coasts of Morocco." South Asian Journal of Experimental Biology 1, no. 2 (April 24, 2011): 101–6. http://dx.doi.org/10.38150/sajeb.1(2).p101-106.

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During the monitoring program of phycotoxins conducted in 2005 and 2006, lipophilic shell fish toxins (LSTs) are involved in shellfish toxicity phenomena in the South Atlantic Moroccan coasts (Dakhla region). Toxicity was assessed by the traditional mouse bioassay (MBA); the content and the nature of the toxic components were established through Liquid chromatography (LC) coupled with mass spectrometry (MS). The ‘traditional’ DSP toxins group, okadaic acid (OA) and dinophysitoxins (DTXs) and their associated esters were exclusives contaminants of Dakhla’s shellfish (mussels, cockles, oysters and solen). Pectenotoxins, yessotoxins, and azaspiracids were not detected during this study. A survey of the phytoplankton community in the surrounding seawater revealed the presence of several potentially toxic species from the Dinophysis genus.
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30

Zhaoxin, Li. "Metabolism of pectenotoxins in brown crabs Cancer pagurus fed blue mussels Mytilus edulis." Journal of Venomous Animals and Toxins including Tropical Diseases 14, no. 3 (2008): 555. http://dx.doi.org/10.1590/s1678-91992008000300018.

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31

Ares, Isabel, Carmen Louzao, Begona Espina, Mercedes Vieytes, Christopher Miles, Takeshi Yasumoto, and Luis Botana. "Lactone Ring of Pectenotoxins: a Key Factor for their Activity on Cytoskeletal Dynamics." Cellular Physiology and Biochemistry 19, no. 5-6 (2007): 283–92. http://dx.doi.org/10.1159/000100647.

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32

Likumahua, Sem, M. Karin de Boer, Bernd Krock, Willem M. Tatipatta, Malik S. Abdul, and Anita G. J. Buma. "Co-occurrence of pectenotoxins and Dinophysis miles in an Indonesian semi-enclosed bay." Marine Pollution Bulletin 185 (December 2022): 114340. http://dx.doi.org/10.1016/j.marpolbul.2022.114340.

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33

Salas, Rafael, and Dave Clarke. "Review of DSP Toxicity in Ireland: Long-Term Trend Impacts, Biodiversity and Toxin Profiles from a Monitoring Perspective." Toxins 11, no. 2 (January 22, 2019): 61. http://dx.doi.org/10.3390/toxins11020061.

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The purpose of this work is to review all the historical monitoring data gathered by the Marine Institute, the national reference laboratory for marine biotoxins in Ireland, including all the biological and chemical data from 2005 to 2017, in relation to diarrheic shellfish poisoning (DSP) toxicity in shellfish production. The data reviewed comprises over 25,595 water samples, which were preserved in Lugol’s iodine and analysed for the abundance and composition of marine microalgae by light microscopy, and 18,166 records of shellfish flesh samples, which were analysed using LC-MS/MS for the presence and concentration of the compounds okadaic acid (OA), dinophysistoxins-1 (DTX-1), dinophysistoxins-2 (DTX-2) and their hydrolysed esters, as well as pectenotoxins (PTXs). The results of this review suggest that DSP toxicity events around the coast of Ireland occur annually. According to the data reviewed, there has not been an increase in the periodicity or intensity of such events during the study period. Although the diversity of the Dinophysis species on the coast of Ireland is large, with 10 species recorded, the two main species associated with DSP events in Ireland are D. acuta and D. acuminata. Moreover, the main toxic compounds associated with these species are OA and DTX-2, but concentrations of the hydrolysed esters are generally found in higher amounts than the parent compounds in the shellfish samples. When D. acuta is dominant in the water samples, the DSP toxicity increases in intensity, and DTX-2 becomes the prevalent toxin. Pectenotoxins have only been analysed and reported since 2012, and these compounds had not been associated with toxic events in Ireland; however, in 2014, concentrations of these compounds were quantitated for the first time, and the data suggest that this toxic event was associated with an unusually high number of observations of D. tripos that year. The areas of the country most affected by DSP outbreaks are those engaging in long-line mussel (Mytilus edulis) aquaculture.
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34

de la Iglesia, P., and A. Gago-Martínez. "Determination of yessotoxins and pectenotoxins in shellfish by capillary electrophoresis-electrospray ionization-mass spectrometry." Food Additives & Contaminants: Part A 26, no. 2 (February 2009): 221–28. http://dx.doi.org/10.1080/02652030802290522.

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35

Miles, Christopher Owen, Alistair L. Wilkins, Allan D. Hawkes, Dwayne J. Jensen, Andrew I. Selwood, Veronica Beuzenberg, A. Lincoln MacKenzie, Janine M. Cooney, and Patrick T. Holland. "Isolation and identification of pectenotoxins-13 and -14 from Dinophysis acuta in New Zealand." Toxicon 48, no. 2 (August 2006): 152–59. http://dx.doi.org/10.1016/j.toxicon.2006.04.005.

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36

Krock, Bernd, Carmen Gloria Seguel, Katherinne Valderrama, and Urban Tillmann. "Pectenotoxins and yessotoxin from Arica Bay, North Chile as determined by tandem mass spectrometry." Toxicon 54, no. 3 (September 2009): 364–67. http://dx.doi.org/10.1016/j.toxicon.2009.04.013.

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37

Butler, Suzanne C., Christopher O. Miles, Amna Karim, and Michael J. Twiner. "Inhibitory effects of pectenotoxins from marine algae on the polymerization of various actin isoforms." Toxicology in Vitro 26, no. 3 (April 2012): 493–99. http://dx.doi.org/10.1016/j.tiv.2011.12.015.

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38

Li, Zhaoxin. "Metabolism of pectenotoxins in brown crabs Cancer pagurus fed with blue mussels Mytilus edulis." Chinese Journal of Oceanology and Limnology 27, no. 3 (September 2009): 468–72. http://dx.doi.org/10.1007/s00343-009-9147-6.

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39

Awakura, Daisuke, Kenshu Fujiwara, and Akio Murai. "ChemInform Abstract: Synthetic Studies on Pectenotoxins: Synthesis of the Common C8-C18 THF Fragment." ChemInform 32, no. 13 (March 27, 2001): no. http://dx.doi.org/10.1002/chin.200113238.

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40

Evans, David A., Hemaka A. Rajapakse, and Dirk Stenkamp. "Asymmetric Syntheses of Pectenotoxins-4 and -8, Part I: Synthesis of the C1–C19 Subunit." Angewandte Chemie International Edition 41, no. 23 (December 2, 2002): 4569–73. http://dx.doi.org/10.1002/1521-3773(20021202)41:23<4569::aid-anie4569>3.0.co;2-v.

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41

Fux, Elie, Sonsoles Gonzalez-Gil, Michel Lunven, Patrick Gentien, and Philipp Hess. "Production of diarrhetic shellfish poisoning toxins and pectenotoxins at depths within and below the euphotic zone." Toxicon 56, no. 8 (December 2010): 1487–96. http://dx.doi.org/10.1016/j.toxicon.2010.09.007.

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42

Kouridaki, Antonia, Tamsyn Montagnon, Maria Tofi, and Georgios Vassilikogiannakis. "Photooxidations of 2-(γ,ε-Dihydroxyalkyl) Furans in Water: Synthesis of DE-Bicycles of the Pectenotoxins." Organic Letters 14, no. 9 (April 19, 2012): 2374–77. http://dx.doi.org/10.1021/ol3007937.

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43

Kemppainen, Eeva K., Gokarneswar Sahoo, Arto Valkonen, and Petri M. Pihko. "Mukaiyama–Michael Reactions with Acrolein and Methacrolein: A Catalytic Enantioselective Synthesis of the C17–C28 Fragment of Pectenotoxins." Organic Letters 15, no. 18 (September 5, 2013): 4916. http://dx.doi.org/10.1021/ol402460b.

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44

Vassilikogiannakis, Georgios, Ioanna Alexopoulou, Maria Tofi, and Tamsyn Montagnon. "Singlet oxygen initiated cascade transformation of a simple difuran into the key ABC-ring motif of the pectenotoxins." Chem. Commun. 47, no. 1 (2011): 259–61. http://dx.doi.org/10.1039/c0cc01341b.

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Kemppainen, Eeva K., Gokarneswar Sahoo, Arto Valkonen, and Petri M. Pihko. "Mukaiyama–Michael Reactions with Acrolein and Methacrolein: A Catalytic Enantioselective Synthesis of the C17–C28 Fragment of Pectenotoxins." Organic Letters 14, no. 4 (February 2012): 1086–89. http://dx.doi.org/10.1021/ol203486p.

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46

Alcántara-Rubira, Alex, Víctor Bárcena-Martínez, Maribel Reyes-Paulino, Katherine Medina-Acaro, Lilibeth Valiente-Terrones, Angélica Rodríguez-Velásquez, Rolando Estrada-Jiménez, and Omar Flores-Salmón. "First Report of Okadaic Acid and Pectenotoxins in Individual Cells of Dinophysis and in Scallops Argopecten purpuratus from Perú." Toxins 10, no. 12 (November 23, 2018): 490. http://dx.doi.org/10.3390/toxins10120490.

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Causative species of Harmful Algal Bloom (HAB) and toxins in commercially exploited molluscan shellfish species are monitored weekly from four classified shellfish production areas in Perú (three in the north and one in the south). Okadaic acid (OA) and pectenotoxins (PTXs) were detected in hand-picked cells of Dinophysis (D. acuminata-complex and D. caudata) and in scallops (Argopecten purpuratus), the most important commercial bivalve species in Perú. LC-MS analyses revealed two different toxin profiles associated with species of the D. acuminata-complex: (a) one with OA (0.3–8.0 pg cell−1) and PTX2 (1.5–11.1 pg cell−1) and (b) another with only PTX2 which included populations with different toxin cell quota (9.3–9.6 pg cell−1 and 5.8–9.2 pg cell−1). Toxin results suggest the likely presence of two morphotypes of the D. acuminata-complex in the north, and only one of them in the south. Likewise, shellfish toxin analyses revealed the presence of PTX2 in all samples (10.3–34.8 µg kg−1), but OA (7.7–15.2 µg kg−1) only in the northern samples. Toxin levels were below the regulatory limits established for diarrhetic shellfish poisoning (DSP) and PTXs (160 µg OA kg−1) in Perú, in all samples analyzed. This is the first report confirming the presence of OA and PTX in Dinophysis cells and in shellfish from Peruvian coastal waters.
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47

Villar-González, Adriano, María Luisa Rodríguez-Velasco, and Ana Gagoo-Martínez. "Determination of Lipophilic Toxins by LC/MS/MS: Single-Laboratory Validation." Journal of AOAC INTERNATIONAL 94, no. 3 (May 1, 2011): 909–22. http://dx.doi.org/10.1093/jaoac/94.3.909.

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Abstract An LC/MS/MS method has been developed, assessed, and intralaboratory-validated for the analysis of the lipophilic toxins currently regulated by European Union legislation: okadaic acid (OA) and dinophysistoxins 1 and 2, including their ester forms; azaspiracids 1, 2, and 3; pectenotoxins 1 and 2; yessotoxin (YTX), and the analogs 45 OH-YTX, Homo YTX, and 45 OH-Homo YTX; as well as for the analysis of 13-desmetil-spirolide C. The method consists of duplicate sample extraction with methanol and direct analysis of the crude extract without further cleanup or concentration. Ester forms of OA and dinophysistoxins are detected as the parent ions after alkaline hydrolysis of the extract. The validation process of this method was performed using both fortified and naturally contaminated samples, and experiments were designed according to International Organization for Standardization, International Union of Pure and Applied Chemistry, and AOAC guidelines. With the exception of YTX in fortified samples, RSDr below 15% and RSDR were below 25%. Recovery values were between 77 and 95%, and LOQs were below 60 μg/kg. These data together with validation experiments for recovery, selectivity, robustness, traceability, and linearity, as well as uncertainty calculations, are presented in this paper.
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48

Matsushima, Ryoji, Hajime Uchida, Satoshi Nagai, Ryuichi Watanabe, Michiya Kamio, Hiroshi Nagai, Masaki Kaneniwa, and Toshiyuki Suzuki. "Assimilation, Accumulation, and Metabolism of Dinophysistoxins (DTXs) and Pectenotoxins (PTXs) in the Several Tissues of Japanese Scallop Patinopecten yessoensis." Toxins 7, no. 12 (December 1, 2015): 5141–54. http://dx.doi.org/10.3390/toxins7124870.

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49

Kim, Mungi, Seongjin Hong, Young Kyun Lim, Jihyun Cha, Jiyun Gwak, Youngnam Kim, Seong-Ah An, Hee-Seok Lee, and Seung Ho Baek. "Spatiotemporal distribution characteristics of yessotoxins and pectenotoxins in phytoplankton and shellfish collected from the southern coast of South Korea." Marine Pollution Bulletin 180 (July 2022): 113776. http://dx.doi.org/10.1016/j.marpolbul.2022.113776.

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50

Díaz, Patricio A., Gonzalo Álvarez, Gemita Pizarro, Juan Blanco, and Beatriz Reguera. "Lipophilic Toxins in Chile: History, Producers and Impacts." Marine Drugs 20, no. 2 (February 4, 2022): 122. http://dx.doi.org/10.3390/md20020122.

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A variety of microalgal species produce lipophilic toxins (LT) that are accumulated by filter-feeding bivalves. Their negative impacts on human health and shellfish exploitation are determined by toxic potential of the local strains and toxin biotransformations by exploited bivalve species. Chile has become, in a decade, the world’s major exporter of mussels (Mytilus chilensis) and scallops (Argopecten purpuratus) and has implemented toxin testing according to importing countries’ demands. Species of the Dinophysis acuminata complex and Protoceratium reticulatum are the most widespread and abundant LT producers in Chile. Dominant D. acuminata strains, notwithstanding, unlike most strains in Europe rich in okadaic acid (OA), produce only pectenotoxins, with no impact on human health. Dinophysis acuta, suspected to be the main cause of diarrhetic shellfish poisoning outbreaks, is found in the two southernmost regions of Chile, and has apparently shifted poleward. Mouse bioassay (MBA) is the official method to control shellfish safety for the national market. Positive results from mouse tests to mixtures of toxins and other compounds only toxic by intraperitoneal injection, including already deregulated toxins (PTXs), force unnecessary harvesting bans, and hinder progress in the identification of emerging toxins. Here, 50 years of LST events in Chile, and current knowledge of their sources, accumulation and effects, are reviewed. Improvements of monitoring practices are suggested, and strategies to face new challenges and answer the main questions are proposed.
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