Purification and characterization of saxitoxin from Mytilus chilensis of southern Chile

D. P. Rubio; L. G. Roa; D. A. Soto; F. J. Velasquez; N. A. Gregorcic; J. A. Soto; M. C. Martinez; A. M. Kalergis; A. E. Vasquez

doi:10.1016/j.toxicon.2015.09.045

Purification and characterization of saxitoxin from Mytilus chilensis of southern Chile

D. P. Rubio, L. G. Roa, D. A. Soto, F. J. Velasquez, N. A. Gregorcic, J. A. Soto, M. C. Martinez, A. M. Kalergis, A. E. Vasquez

Research output: Contribution to journal › Article › peer-review

7 Citations (Scopus)

Abstract

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.

Original language	English
Pages (from-to)	147-153
Number of pages	7
Journal	Toxicon
Volume	108
DOIs	https://doi.org/10.1016/j.toxicon.2015.09.045
Publication status	Published - 15 Dec 2015
Externally published	Yes

Keywords

Harmful algal blooms
HPLC
Mylitus chilensis
Paralytic shellfish poison
Saxitoxin

ASJC Scopus subject areas

Toxicology

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10.1016/j.toxicon.2015.09.045

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title = "Purification and characterization of saxitoxin from Mytilus chilensis of southern Chile",

abstract = "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.",

keywords = "Harmful algal blooms, HPLC, Mylitus chilensis, Paralytic shellfish poison, Saxitoxin",

author = "Rubio, {D. P.} and Roa, {L. G.} and Soto, {D. A.} and Velasquez, {F. J.} and Gregorcic, {N. A.} and Soto, {J. A.} and Martinez, {M. C.} and Kalergis, {A. M.} and Vasquez, {A. E.}",

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year = "2015",

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doi = "10.1016/j.toxicon.2015.09.045",

language = "English",

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AU - Rubio, D. P.

AU - Roa, L. G.

AU - Soto, D. A.

AU - Velasquez, F. J.

AU - Gregorcic, N. A.

AU - Soto, J. A.

AU - Martinez, M. C.

AU - Kalergis, A. M.

AU - Vasquez, A. E.

PY - 2015/12/15

Y1 - 2015/12/15

N2 - 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.

AB - 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.

KW - Harmful algal blooms

KW - HPLC

KW - Mylitus chilensis

KW - Paralytic shellfish poison

KW - Saxitoxin

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JO - Toxicon

JF - Toxicon

ER -

Purification and characterization of saxitoxin from Mytilus chilensis of southern Chile

Abstract

Keywords

ASJC Scopus subject areas

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