石墨烯-管尖固相萃取-液相色谱-串联质谱法测定贝类中10种脂溶性贝类毒素

doi:10.3724/SP.J.1123.2018.11042

色谱 ›› 2019, Vol. 37 ›› Issue (5): 505-511.DOI: 10.3724/SP.J.1123.2018.11042

石墨烯-管尖固相萃取-液相色谱-串联质谱法测定贝类中10种脂溶性贝类毒素

杨霄^1,3, 黄华伟^1,3, 伍远安^1,2, 万译文³, 李小玲³, 黄向荣^1,3

1. 湖南省水产科学研究所, 湖南长沙 410153;
2. 水产高效健康生产湖南省协同创新中心, 湖南常德 415000;
3. 农业部渔业产品质量监督检验测试中心(长沙), 湖南长沙 410153

收稿日期:2018-11-29 出版日期:2019-05-08 发布日期:2015-03-23
通讯作者: 黄向荣,E-mail:hns-11@126.com
基金资助:
农产品质量安全监管专项经费项目（181821301092362）；湖南省科技重大专项（2017NK1030）.

Graphene-based pipette tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish

YANG Xiao^1,3, HUANG Huawei^1,3, WU Yuan'an^1,2, WAN Yiwen³, LI Xiaoling³, HUANG Xiangrong^1,3

1. Hunan Fisheries Science Institute, Changsha 410153, China;
2. Collaborative Innovation Center for Efficient and Health Production of Fisheries in Hunan, Changde 415000, China;
3. Fishery Products Quality Supervision and Testing Center, Ministry of Agriculture, Changsha 410153, China

Received:2018-11-29 Online:2019-05-08 Published:2015-03-23
Supported by:
Special Fund Project for Quality and Safety Supervision of Agricultural Products (No. 181821301092362); Science and Technology Major Project of Hunan Province (No. 2017NK1030).

摘要/Abstract

摘要：

以石墨烯为吸附剂，制作了石墨烯-管尖固相萃取装置，结合液相色谱-串联质谱，建立了一种同时测定贝类中10种脂溶性贝类毒素的方法。实验对提取剂、石墨烯的用量、淋洗剂的种类和用量、洗脱剂的种类和用量等实验参数进行了详细优化。在最优的实验条件下，10种脂溶性贝类毒素在各自相应浓度范围内线性良好，相关系数均大于0.99，方法检出限（LOD）和定量限（LOQ）分别在0.1~1.1 μg/kg和0.3~3.2 μg/kg之间；对阴性牡蛎样品进行3个水平的加标回收实验，10种脂溶性贝类毒素的回收率在72.0%~101.2%之间，相对标准偏差小于15%。结果表明，该方法灵敏度高，操作简单高效，适用于贝类水产品中脂溶性贝类毒素的检测分析。

关键词: 贝类, 管尖固相萃取, 石墨烯, 液相色谱-串联质谱, 脂溶性贝类毒素

Abstract:

A method for the simultaneous determination of ten lipophilic shellfish toxins was established based on graphene-based pipette tip solid-phase extraction (G-PT-SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The factors influencing the extraction efficiency, including the types of extractants, the amount of graphene, the types and volumes of washing and eluent solvents, were optimized in detail. Under the optimal conditions, the calibration curves showed linear relationships between the LC peak areas of the selected ion-pairs and the mass concentrations of the ten lipophilic shellfish toxins with correlation coefficients >0.99. The limits of detection (LODs) and the limits of quantification (LOQs) of the method were 0.1-1.1 μg/kg and 0.3-3.2 μg/kg, respectively. The recoveries of the ten lipophilic shellfish toxins spiked in blank oyster at three levels ranged from 72.0% to 101.2% with relative standard deviations <15%. The method is sensitive, simple, and effective, and is suitable for the determination of the lipophilic shellfish toxins in shellfish products.

Key words: graphene, lipophilic shellfish toxins, liquid chromatography-tandem mass spectrometry (LC-MS/MS), pipette tip solid-phase extraction, shellfish

中图分类号:

O658

杨霄, 黄华伟, 伍远安, 万译文, 李小玲, 黄向荣. 石墨烯-管尖固相萃取-液相色谱-串联质谱法测定贝类中10种脂溶性贝类毒素[J]. 色谱, 2019, 37(5): 505-511.

YANG Xiao, HUANG Huawei, WU Yuan'an, WAN Yiwen, LI Xiaoling, HUANG Xiangrong. Graphene-based pipette tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish[J]. Chinese Journal of Chromatography, 2019, 37(5): 505-511.

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石墨烯-管尖固相萃取-液相色谱-串联质谱法测定贝类中10种脂溶性贝类毒素

Graphene-based pipette tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish

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