基于 3D 石墨烯的超声辅助磁固相萃取选择性测定食品中的咖啡因。
Selective determination of caffeine in foods with 3D-graphene based ultrasound-assisted magnetic solid phase extraction.
机构信息
Department of Chemistry, University of Guilan, University Campus 2, Rasht, Iran; Research Laboratory, SumTech Co. (Newsaad Hygienic and Cosmetics), Pardis St., Sanaat 1 BLV., 1st Intrance, Rasht Industrial Area, Iran.
Department of Chemistry, University of Guilan, University Campus 2, Rasht, Iran; Department of Chemistry, Faculty of Science, University of Guilan, Rasht, Iran.
出版信息
Food Chem. 2018 Oct 1;262:206-214. doi: 10.1016/j.foodchem.2018.04.035. Epub 2018 Apr 13.
An efficient method was applied for extraction of caffeine in food samples. Three-dimensional graphene-FeO (3D-G-FeO) nanoparticles was successfully synthesized and used as adsorbent in magnetic solid phase extraction (MSPE) step. The properties of synthesized adsorbent were characterized by fourier-transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Raman spectroscopy, Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) methods. The influence of main parameters of extraction procedure such as ultrasound parameter, amount of nanoparticles, pH, salt concentration and desorption condition were investigated and optimized. Under the optimized experimental conditions, the figure of merit results showed excellent linear dynamic range (LDR) of 0.5-500 µg mL, with determination coefficient (R) higher than 0.996 and limit of detection (LOD) of 0.1 µg mL. Intra- and inter-day relative standard deviations (RSDs) were less than 5.9 and 7.1%, respectively. The method was successfully applied for determination of caffeine in different food samples.
一种高效的方法被应用于食品样品中咖啡因的提取。三维石墨烯 - FeO（3D-G-FeO）纳米粒子被成功合成，并用作磁固相萃取（MSPE）步骤中的吸附剂。通过傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、振动样品磁强计（VSM）、X 射线衍射（XRD）、拉曼光谱、BET 和 Barrett-Joyner-Halenda（BJH）方法对合成吸附剂的性质进行了表征。考察并优化了萃取过程的主要参数，如超声参数、纳米粒子用量、pH 值、盐浓度和洗脱条件。在优化的实验条件下，优点因子结果显示出优异的线性动态范围（LDR）为 0.5-500 µg mL，相关系数（R）高于 0.996，检测限（LOD）为 0.1 µg mL。日内和日间相对标准偏差（RSD）分别小于 5.9%和 7.1%。该方法成功应用于不同食品样品中咖啡因的测定。
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