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免疫亲和柱净化-液相色谱-串联质谱法测定海洋生物中河豚毒素
引用本文:严忠雍,张小军,李奇富,王莹,柳家鹏,龙举,祝银,杨会成.免疫亲和柱净化-液相色谱-串联质谱法测定海洋生物中河豚毒素[J].分析化学,2015(2):277-281.
作者姓名:严忠雍  张小军  李奇富  王莹  柳家鹏  龙举  祝银  杨会成
作者单位:1. 浙江省海洋水产研究所,舟山316021; 浙江省海洋渔业资源可持续利用技术研究重点实验室,舟山316021
2. 江苏美正生物科技有限公司,无锡,214135
3. 浙江省海洋开发研究院,舟山,316021
基金项目:国家十二五科技支撑项目,浙江省自然科学基金项目(No. LQ13C200004)资助This work was supported by the Twelfth Five-Year National Science and Technology Support Program
摘    要:建立了海洋生物中河豚毒素的免疫亲和柱净化-液相色谱-串联质谱分析方法。采用1%乙酸-甲醇提取样品,提取液通过磷酸盐缓冲液稀释,调节至pH 7~8,经免疫亲和柱富集和净化后,LC-MS/MS测定,外标法定量。在ACQUITY UPLC BEH Amide亲水柱上进行分离,流动相为乙腈和含有0.1%甲酸的5 mmol/L乙酸铵溶液,梯度洗脱,电喷雾正离子多反应模式监测。河豚毒素在0.3~20.0μg/L线性范围内,相关系数大于0.997,定量限为0.3μg/kg,回收率为88.7%~102.3%,相对标准偏差2.0%~6.4%。本方法重现性好、灵敏度高,适用于海洋生物中河豚毒素的测定。

关 键 词:免疫亲和柱  液相色谱-串联质谱  海洋生物  河豚毒素

Determination of Tetrodotoxin in Marine Organisms by High Performance Liquid Chromatography-Mass Spectrometry and Cleaned up by Immunoaffinity Column
YAN Zhong-Yong,ZHANG Xiao-Jun,LI Qi-Fu,WANG Ying,LIU Jia-Peng,LONG Ju,ZHU Yin,YANG Hui-Cheng.Determination of Tetrodotoxin in Marine Organisms by High Performance Liquid Chromatography-Mass Spectrometry and Cleaned up by Immunoaffinity Column[J].Chinese Journal of Analytical Chemistry,2015(2):277-281.
Authors:YAN Zhong-Yong  ZHANG Xiao-Jun  LI Qi-Fu  WANG Ying  LIU Jia-Peng  LONG Ju  ZHU Yin  YANG Hui-Cheng
Institution:YAN Zhong-Yong;ZHANG Xiao-Jun;LI Qi-Fu;WANG Ying;LIU Jia-Peng;LONG Ju;ZHU Yin;YANG Hui-Cheng;Marine Fisheries Research Institute of Zhejiang;Key lab of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang;Jiangsu Meizheng Biotechnology Co.,Ltd.;Zhejiang Marine Development Research Institute;
Abstract:
Keywords:Immunoaffinity column  High performance liquid chromatography-mass spectrometry  Marine organisms  Tetrodotoxin
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