Asfaram Arash, Ghaedi Mehrorang, Dashtian Kheibar
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Ultrason Sonochem. 2017 Jan;34:561-570. doi: 10.1016/j.ultsonch.2016.06.033. Epub 2016 Jun 23.
Magnetite (FeO nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-FeO-GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-FeO-NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV-Vis (UA-DMSPME-UV-Vis) detection method. Plackett-Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-FeO-NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-FeO-NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6mg, 4.0min and 180μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8-6000ngmL with a Limit of detection (LOD) of 1.377ngmL, limit of quantification (LOQ) 4.591ngmL and precision (<3.50% RSD). The recovery of GA in urine, human plasma and water samples within the range of 92.3-100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application.
以磁铁矿（FeO纳米颗粒（NPs））HKUST-1金属有机框架（MOF）复合材料为载体，使用乙烯基三甲氧基硅烷（VTMOS）作为交联剂，用于制备没食子酸印迹聚合物（HKUST-1-MOF-FeO-GA-MIP）的表面印迹。随后，通过傅里叶变换红外光谱（FT-IR）、X射线衍射（XRD）和场发射扫描电子显微镜（FE-SEM）分析对HKUST-1-MOF-FeO-NPs-GA-MIP进行表征，并将其应用于通过紫外可见光谱（UV-Vis）检测法对没食子酸（GA）进行快速、选择性和灵敏的超声辅助分散磁性固相微萃取（UA-DMSPME-UV-Vis）。根据期望函数（DF）的Plackett-Burman设计（PBD）和中心复合设计（CCD）表明了萃取因素中涡旋（混合）时间（分钟）、超声时间（分钟）、温度（°C）、洗脱液体积（升）、pH值以及HKUST-1-MOF-FeO-NPs-GA-MIP质量（毫克）等显著变量及其对响应的贡献。最佳条件和数值对应于pH值、HKUST-1-MOF-FeO-NPs-GA-MIP质量、超声时间和洗脱液体积，分别设定为3.0、1.6毫克、4.0分钟和180微升。GA的平均回收率（ER%）为98.13%，期望度为0.997，而本方法具有最佳的操作性能，如宽线性范围8 - 6000纳克/毫升，检测限（LOD）为1.377纳克/毫升，定量限（LOQ）为4.591纳克/毫升，精密度（<3.50%相对标准偏差）。GA在尿液、人血浆和水样中的回收率在92.3 - 100.6%范围内，这有力地支持了本方法在实际样品分析中的高适用性，使该方法有望得到进一步应用。
