多壁碳纳米管固相萃取-超高效液相色谱串联质谱法测定织纹螺中河豚毒素  

Determination of tetrodotoxin in Nassarius by ultra high performance liquid chromatography-tandem mass spectrometry with multi-walled carbon nanotubes purification

作　　者：孙博伦 王旭峰[2] 李来好[2] 赵东豪[2] 王强[2] 黎智广[2] 蔡楠[2] 关婉琪 SUN Bolun;WANG Xufeng;LI Laihao;ZHAO Donghao;WANG Qiang;LI Zhiguang;CAI Nan;GUAN Wanqi(Zhejiang Ocean University,Zhoushan 316021,China;Key Laboratory of Aquatic Product Processing,Ministry of Agriculture and Rural Affairs;Guangdong Provincial Key Laboratory of Fishery Ecology Environment;South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510300,China)

机构地区：[1]浙江海洋大学食品与医药学院,浙江舟山316022 [2]中国水产科学研究院南海水产研究所,农业农村部水产品加工重点实验室,广东省渔业生态环境重点开放实验室,广东广州510300

出　　处：《南方水产科学》2018年第5期103-108,共6页South China Fisheries Science

基　　金：中国水产科学研究院中央级公益性科研院所基本科研业务费专项资金(2016HY-ZD1102,2017HY-YJ0203);国家自然科学基金项目(31571869)。

摘　　要：建立了多壁碳纳米管(MWCNTs)固相萃取-超高效液相色谱串联质谱法(UPLC-MS/MS)测定织纹螺中河豚毒素(TTX)的方法,样品用1%乙酸甲醇溶液提取,调节pH至8.5~9.0后,采用碳纳米管净化处理后上机测定。以乙腈和0.1%甲酸水溶液为流动相,经Amide柱梯度洗脱,以电喷雾离子源正离子模式,多反应监测(MRM)测定,外标法定量。在0.3~50 ng·mL^(–1)质量浓度范围内,相关系数(R)大于0.999,加标回收率为83.7%~91.4%,相对标准偏差为2.3%~8.6%,检测限和定量限分别为0.3μg·kg^(–1)和1μg·kg^(–1)。该方法适用于织纹螺中TTX的检测。A sensitive and reliable method for determination of tetrodotoxin(TTX)in Nassarius was established using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted by 1%acetic acid-methanol solution,then the pH value was adjusted to 8.5?9.0.After purification with multi-walled carbon nanotubes(MWCNTs),the sample was subjected to an analytical procedure.The mobile phase containing acetonitrile and 0.1%formic acid solution with a linear gradient elution was utilized to separate TTX on an Amide column.The quantitative analysis was carried out with an external standard method in the multiple reaction monitoring mode using positive electrospray ionization.The calibration curve for TTX was linear(R>0.999)from 0.3 ng·mL^–1 to 50 ng·mL^–1.The recoveries were 83.7%?91.4%with the RSDs of 2.3%?8.6%.The limits of detection and quantification were 0.3μg·kg^–1 and 1μg·kg^–1,respectively.This method is suitable for determination of TTX in Nassarius.

关 键 词：河豚毒素 织纹螺 多壁碳纳米管 液相色谱-质谱联用检测法 固相萃取 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]