基于金属有机框架/氧化石墨烯半自动化管尖固相萃取-高效液相色谱法测定食品中的槲皮素  

Combination of Pipette Tip Solid Phase Extraction and High Performance Liquid Chromatography for Determination of Quercetin in Food Samples based on the Metal-Organic Framework/Graphene Oxide as Highly Efficient Sorbent

作　　者：王露[1] 王丹丹 宋鑫[1] 连中宇 冯晓青[1] 杨鹏飞[1] 邢亚东[1] WANG Lu;WANG Dandan;SONG Xin;LIAN Zhongyu;FENG Xiaoqing;YANG Pengfei;XING Yadong(Huaian Center for Disease Control and Prevention,Huaian,Jiangsu 223001)

机构地区：[1]淮安市疾病预防控制中心,江苏淮安223001

出　　处：《分析科学学报》2024年第5期546-552,共7页Journal of Analytical Science

基　　金：淮安市科技计划项目(HAB202222,HAB202340);淮安市突发公共卫生事件应急检测重点实验室(HAP201906);江苏省预防医学研究课题(Ym2023022)。

摘　　要：基于水热法制备了金属有机框架/氧化石墨烯(Cu-MOF/GO)复合材料为管尖固相萃取吸附剂,结合高效液相色谱法建立了食品中槲皮素的分析方法。利用傅里叶变换红外光谱、X射线衍射仪和扫描电子显微镜对Cu-MOF/GO复合材料进行了表征。实验优化了样品pH、吸附材料用量、样品流速、洗脱剂种类及体积、样品体积等实验条件。结果显示,20mg吸附材料可在25min内完成溶液中(pH6.0)96%槲皮素的吸附,以1mL的0.1%甲酸-甲醇洗脱槲皮素,在最佳实验条件下,槲皮素在0.1~120μg/L范围内线性关系良好,相关系数为0.9993,检出限为0.066μg/L。实际样品的回收率为87.4%~109.5%,相对标准偏差为1.7%~4.9%。该复合材料对槲皮素的饱和吸附容量为196.0mg/g,且可多次重复使用。所建立方法操作简便、灵敏度高、准确度好,为不同食品中槲皮素的检测提供了新方法。In this study,Cubased metalorganic framework/graphene oxide(CuMOF/GO)nanocomposite was used as a sorbent for the pipette tip microsolid phase extraction(PTμSPE)of quercetin from food samples.The metalorganic framework/graphene oxide composites were prepared by hydrothermal method.The composites were characterized by Fourier transform infrared spectroscopy,Xray diffraction and scanning electron microscopy.The adsorption parameters including solution pH,flowrate of sample,adsorbent amount,volume of sample,elution solvent and its volume were optimized by batch adsorption experiment.Twenty mg adsorption material could adsorb 96%of quercetin in samples(pH 6.0)within 25 min,and 1 mL 0.1%methanoic acidmethanol could fully desorb the target.Under the optimized extraction conditions,there was a good linearity in the range of 0.1-120μg/L quercetin with a limits of detection of 0.066μg/L.The average recoveries for quercetin were between 87.4%and 109.5%with RSD of 1.7%-4.9%in spiked food samples.The saturated adsorption capacity of the adsorption material was 196.0 mg/g,which could be reused for many times.The results showed that the prepared adsorbent provided desirable adsorption capacity of quercetin,demonstrating great potential in the detection of quercetin in complex food matrices.

关 键 词：金属有机骨架/氧化石墨烯 半自动化管尖固相萃取 槲皮素 高效液相色谱 

分 类 号：O657.72[理学—分析化学]