Rapid Determination of Tetrodotoxin in Human Plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作     者：CHEN Weizhu ZHANG Yiping SUN Jipeng XIE Quanling HONG Zhuan YI Ruizao 无

作者机构：Third Institute of OceanographyState Oceanic AdministrationXiamen 361005P.R.China Engineering Research Center of Marine Biological Resource Comprehensive UtilizationState Oceanic AdministrationXiamen 361005P.R.China Fujian Collaborative Innovation Center for Exploitation and Utilization of Marine Biological Resources Xiamen 361005P.R.China 

出 版 物：《Chemical Research in Chinese Universities》 (高等学校化学研究（英文版）)

年 卷 期：2018年第34卷第6期

页      面：905-911页

核心收录：

学科分类：0710[理学-生物学] 071010[理学-生物化学与分子生物学] 081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 082304[工学-载运工具运用工程] 080204[工学-车辆工程] 0703[理学-化学] 0802[工学-机械工程] 0823[工学-交通运输工程] 

基　　金：Supported by the National Key Research and Development Program of China(No.2016YFF0201104) the Construction of Public Service Platform for Research and Test of Marine Pilot Technology of China(No.Bhsfs009) the Project of Xiamen Southern oceanographic Center,China(No.16PFW008SF15) 

主　　题：Tetrodotoxin(TTX) 11-DeoxyTTX Ultra performance liquid chromatography(UPLC)coupled with tandem mass spectrometry(MS/MS) Plasma Protein precipitation 

摘      要：A sensitive analytical method was developed to determine tetrodotoxin（TTX） in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography（UPLC） analysis coupled with tandem mass spectrometry（MS/MS） using 11-deoxytetrodotoxin（11-deoxyTTX） as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions（i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX） in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.