PDF《石墨烯 ⁃管尖固相萃取 ⁃液相色谱 ⁃串联质谱法》

2019 年5月Vol.

37 No.5 May

2019 Chinese Journal of Chromatography 505~511 研究论文 DOI: 10.3724/ SP.J.1123.2018.11042 ?收稿日期:2018?11?29 ?通讯联系人.E?mail:hns?11@ 126.com. 基金项目: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). Foundation item: Special Fund Project for Quality and Safety Supervision of Agricultural Products (No. 181821301092362);

Science and Technology Major Project of Hunan Province (No. 2017NK1030). 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) 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:石墨烯;

管尖固相萃取;

液相色谱?串联质谱;

脂溶性贝类毒素;

贝类 中图分类号:O658 文献标识码:A 文章编号:1000?8713(2019)05?0505?07 Graphene?based pipette tip solid?phase extraction coupled with liquid chromatography?tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish YANG Xiao1,3 , HUANG Huawei1,3 , WU Yuan'an1,2 , WAN Yiwen3 , LI Xiaoling3 , HUANG Xiangrong1,3? (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) 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 condi? tions, 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 correla? tion 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