title: Development and validation of a high-throughput online solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the detection of gonyautoxins 1&4 and gonyautoxins 2&3 in human urine.
abstract: Paralytic shellfish toxins (PSTs), including gonyautoxins and saxitoxins, are produced by multiple species of microalgae and dinoflagellates, and are bioaccumulated by shellfish and other animals. Human exposure to PSTs typically occurs through ingestion of recreationally harvested contaminated shellfish and results in nonspecific symptomology. Confirmation of exposure to PSTs has often relied on the measurement of saxitoxin, the most toxic congener; however, gonyautoxins (GTXs), the sulfated carbamate derivatives of saxitoxin, may be present in shellfish at higher concentrations. To improve identification of PST exposures, our group has developed an online solid phase extraction hydrophilic interaction liquid chromatography method to identify GTX1-4 in human urine with tandem mass spectrometry. The reportable range varied for each analyte, with all falling within 0.899 and 250 ng/mL in urine with precision <15% and >85% accuracy as determined for all quality control samples. This new online method quantitates GTX1-4 following exposures to PSTs, supporting the work of public health authorities.
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Rebecca
authors.identifier: http://orcid.org/0000-0001-7431-8271
authors.initials: R
authors.lastname: Coleman
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Sharon W
authors.initials: SW
authors.lastname: Lemire
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: William
authors.initials: W
authors.lastname: Bragg
authors.affiliation: National Biodefense Analysis and Countermeasures Center, Fort Detrick, MD, USA.
authors.forename: Alaine
authors.initials: A
authors.lastname: Garrett
authors.affiliation: ORISE Fellow, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Geovannie
authors.initials: G
authors.lastname: Ojeda-Torres
authors.affiliation: Battelle, Atlanta, GA, USA.
authors.forename: Rebekah
authors.initials: R
authors.lastname: Wharton
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Elizabeth
authors.initials: E
authors.lastname: Hamelin
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Jerry
authors.initials: J
authors.lastname: Thomas
authors.affiliation: Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.
authors.forename: Rudolph C
authors.initials: RC
authors.lastname: Johnson
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D057166:High-Throughput Screening Assays / Q000379:methods; D006801:Humans; D057230:Limit of Detection; D016014:Linear Models; D015203:Reproducibility of Results; D012530:Saxitoxin / Q000031:analogs & derivatives* / Q000737:chemistry / Q000302:isolation & purification / Q000652:urine; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D012530:Saxitoxin; C013007:gonyautoxins
keywords: HILIC; gonyautoxin; marine toxins; online SPE; paralytic; saxitoxins