Purification and characterization of saxitoxin from Mytilus chilensis of southern Chile

In the current communication we describe an innovative method to purify saxitoxin (STX), a toxin presents in contaminated muscle of Mylitus chilensis extracted in the southern part of Chile, using a liquid chromatographic methodology based on ionic pairs. The STX was extracted using HCl and treated...

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Bibliographic Details
Published in:	Toxicon (Oxford) Vol. 108; pp. 147 - 153
Main Authors:	Rubio, D.P., Roa, L.G., Soto, D.A., Velasquez, F.J., Gregorcic, N.A., Soto, J.A., Martinez, M.C., Kalergis, A.M., Vasquez, A.E.
Format:	Journal Article
Language:	English
Published:	England Elsevier Ltd 15-12-2015
Subjects:	Ammonium Sulfate - chemistry Animals Cationic Chile Chromatography, High Pressure Liquid - methods Chromatography, Liquid Diethyl ether Harmful algal blooms Hexanes HPLC Hydrochloric Acid - chemistry Liquids Mice Muscles Mylitus chilensis Mytilus - chemistry Mytilus chilensis Paralytic shellfish poison Purification Saxitoxin Saxitoxin - chemistry Saxitoxin - isolation & purification Solid Phase Extraction - methods Tandem Mass Spectrometry Toxins Saxitoxin Harmful algal blooms Paralytic shellfish poison Mylitus chilensis HPLC
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Summary:	In the current communication we describe an innovative method to purify saxitoxin (STX), a toxin presents in contaminated muscle of Mylitus chilensis extracted in the southern part of Chile, using a liquid chromatographic methodology based on ionic pairs. The STX was extracted using HCl and treated with ammonium sulfate following a treatment with trichloroacetic acid and hexane/diethyl ether (97/3). The samples were analyzed by a semi-preparative HPLC in order to collect pure fractions of STX and these fractions were eluted in solid-phase cationic interchange SCX extraction columns. The purified STX was stable and homogeneous and its identity was confirmed by LC–MS–MS, which demonstrated a high quality purification of STX, without presence of analogs such as neosaxitoxin (Neo) and decarbamoyl saxitoxin (dcSTX). The STX biological activity was analyzed in a bioassay in mice model and compared to the standard STX produced by the FDA and no significant differences were observed. •In Chile, most of the intoxications are produced by Paralytic Shellfish Poisoning (PSP), Diarrheic Shellfish Poisoning (DSP) and Amnesic Shellfish Poisoning (ASP), along the Chilean coast.•Saxitoxin is a toxin presents in contaminated muscle of Mylitus chilensis extracted in the southern part of Chile.•STX detection methods in Chile are dependent of STX standard made in other countries.•We purify STX with biological activity similar to standard STX produced by the FDA.
Bibliography:	ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 23
ISSN:	0041-0101 1879-3150
DOI:	10.1016/j.toxicon.2015.09.045