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一种用于检测人尿中膝沟藻毒素1&4和膝沟藻毒素2&3的高通量在线固相萃取-液相色谱-串联质谱法的开发与验证

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.

作者信息

Coleman Rebecca, Lemire Sharon W, Bragg William, Garrett Alaine, Ojeda-Torres Geovannie, Wharton Rebekah, Hamelin Elizabeth, Thomas Jerry, Johnson Rudolph C

机构信息

Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA, USA.

National Biodefense Analysis and Countermeasures Center, Fort Detrick, MD, USA.

出版信息

Biomed Chromatogr. 2017 Sep;31(9). doi: 10.1002/bmc.3954. Epub 2017 Mar 14.

DOI:10.1002/bmc.3954
PMID:28186342
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.

摘要

麻痹性贝类毒素(PSTs),包括膝沟藻毒素和石房蛤毒素,由多种微藻和甲藻产生,并在贝类和其他动物体内生物累积。人类接触PSTs通常是通过食用休闲捕捞的受污染贝类,从而导致非特异性症状。对PSTs暴露的确认通常依赖于对毒性最强的同类物石房蛤毒素的测量;然而,膝沟藻毒素(GTXs),即石房蛤毒素的硫酸化氨基甲酸酯衍生物,在贝类中的浓度可能更高。为了改进对PSTs暴露的识别,我们团队开发了一种在线固相萃取亲水作用液相色谱法,用于通过串联质谱法鉴定人尿液中的GTX1 - 4。每种分析物的报告范围各不相同,在尿液中均落在0.899至250 ng/mL之间,所有质量控制样品的精密度<15%,准确度>85%。这种新的在线方法可在接触PSTs后对GTX1 - 4进行定量,为公共卫生当局的工作提供了支持。

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