作者：杨钰婷1, 王永1, 周柚廷1, 陈杨洁1, 梁立1, 李惠茗2, 刘坤平1
作者单位：1. 成都大学药学院 药食同源植物资源开发四川省高校重点实验室，四川 成都 610106;
2. 成都大学食品与生物工程学院，四川 成都 610106
关键词：石墨烯;固相萃取(SPE);毛细管电泳;联用技术;双酚A
摘要：
制备高比表面积的石墨烯纳米材料，然后将其用做固相萃取(SPE)吸附剂制备石墨烯基SPE小柱。利用所制备的石墨烯基SPE小柱对双酚A（BPA）的高效富集作用并结合毛细管（CE）技术的高效检测能力构建SPE-CE联用分析方法。通过优化实验获取所制备的石墨烯基SPE小柱对BPA的最优萃取条件和最优CE检测条件。在最优条件下，经与商品化的SPE小柱对比，所构建的SPE-CE联用分析方法对BPA在0.05~80 μg/mL范围内表现出良好的线性关系，检出限可达0.02 μg/mL (S/N=3σ)。此外，采用甲醇超声提取和纯水回流提取两种方法提取婴儿奶嘴实际样品中痕量BPA，用所构建的SPE-CE联用分析方法测定婴儿奶嘴实际样品中BPA的迁移量，该方法表现出良好的准确性和精密度，可实现实际样品中痕量BPA的高灵敏快速检测。因此，该文所构建的联用方法可为食品接触材料中痕量组分的分析检测提供可行的思路，具有广阔的应用前景。
Detection of trace bisphenol A in nipple based on graphene solid phase extraction coupled with capillary electrophoresis
YANG Yuting1, WANG Yong1, ZHOU Youting1, CHEN Yangjie1, LIANG Li1, LI Huiming2, LIU Kunping1
1. Key Laboratory of Medicinal and Edible Plants Resources Development of Sichuan Education Department, School of Pharmacy, Chengdu University, Chengdu 610106, China;
2. School of Food and Biological Engineering, Chengdu University, Chengdu 610106, China
Abstract: High specific surface area graphene was first prepared and used as the solid phase extraction (SPE) adsorbent to prepare the graphene based SPE tube. Based on the high efficiency adsorption capacity for bisphenol A (BPA) of graphene and the fine detection ability of capillary electrophoresis (CE), the SPE-CE coupling technique was constructed. Through the optimization of experiment, the optimal SPE experimental condition and CE detection condition was acquired. Under the optimal experimental condition, compared with the commercial SPE tube, the constructed SPE-CE coupling method exhibited fine line relationship between 0.05-80 μg/mL with a detection limit of 0.02 μg/mL (S/N=3σ) for BPA detection. Furthermore, for real infant nipple sample BPA detection, methanol ultrasonic extraction and water reflux extraction were used to extract the trace BPA in infant nipple. Then, the SPE-CE coupling method was used for the detection of BPA migration mass of infant nipple. It shown fine accuracy and precision which exhibited that the constructed SPE-CE coupling method can achieved the fast and sensitive detection of trace BPA in real sample. Thus, this detection strategy provided a feasible approach for trace component in food contacting material and shown wide application prospect.
Keywords: graphene;solid phase extraction (SPE);capillary electrophoresis;coupling technique;bisphenol A
2022, 48(5):65-71 收稿日期: 2020-12-30;收到修改稿日期: 2021-03-27
基金项目: 国家自然基金面上项目（31870078）；第二次青藏高原科学综合科学考察研究项目（2019QZKK020107）
作者简介: 杨钰婷（1995-），女，四川成都市人，硕士研究生，专业方向为分析化学
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