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MgO-ZnO/carbon nanofiber nanocomposite as an adsorbent for ultrasound-assisted dispersive solid-phase microextraction of carbamazepine from wastewater prior to high-performance liquid chromatographic detection
Journal of Analytical Science and Technology ( IF 2.5 ) Pub Date : 2019-07-02 , DOI: 10.1186/s40543-019-0185-1
Malesela William Lekota , K. Mogolodi Dimpe , Philiswa Nosizo Nomngongo

A simple, rapid, and efficient ultrasound-assisted dispersive solid-phase microextraction (UA-DSPME) method was developed for the preconcentration of carbamazepine (CBZ) in wastewater prior to high-performance liquid chromatography coupled with diode array (HPLC-DAD) determination. The carbon nanofibers coated with magnesium oxide-zinc oxide (MgO-ZnO@CNFs) nanocomposite was used as an efficient adsorbent in magnetic dispersive solid-phase microextraction method. The structural and morphological properties of the nanocomposite were characterized by scanning electron microscopy and energy dispersive spectroscopy, transmission electron microscopy, X-ray diffractometer, and Fourier transform infrared spectroscopy. The surface area was investigated using Brunauer–Emmett–Teller. Several factors (such as pH, mass of adsorbent, extraction time, and eluent volume) that affect extraction and preconcentration of CBZ were also assessed and optimized using response surface methodology based on central composite design. Under optimal conditions, the limits of detection (LOD) and quantification were 0.08 μg L−1 and 0.29 μg L−1, respectively. The calibration curve constructed after preconcentration of seven successive standards was linear in the concentration range of 0.3–800 μg L−1 with the correlation coefficient of 0.9922. The intra-day and inter-day precisions expressed in terms of relative standard deviation were 1.4% and 4.2%. A preconcentration factor of 490 was achieved, and the method was applied for the analysis of spiked wastewater. Satisfactory recoveries ranging from 97.8 to 102% were obtained.

中文翻译:

MgO-ZnO/碳纳米纤维纳米复合材料作为吸附剂用于超声辅助分散固相微萃取废水中的卡马西平,然后进行高效液相色谱检测

开发了一种简单、快速、高效的超声辅助分散固相微萃取 (UA-DSPME) 方法,用于在高效液相色谱联用二极管阵列 (HPLC-DAD) 测定之前预浓缩废水中的卡马西平 (CBZ) . 用氧化镁-氧化锌(MgO-ZnO@CNFs)纳米复合材料包覆的碳纳米纤维在磁分散固相微萃取法中用作有效的吸附剂。通过扫描电子显微镜和能量色散光谱、透射电子显微镜、X 射线衍射仪和傅里叶变换红外光谱对纳米复合材料的结构和形态特性进行了表征。使用 Brunauer-Emmett-Teller 研究表面积。几个因素(如 pH、吸附剂质量、提取时间、还使用基于中心复合设计的响应面方法来评估和优化影响 CBZ 提取和预浓缩的(和洗脱液体积)。在最佳条件下,检测限 (LOD) 和定量限分别为 0.08 μg L-1 和 0.29 μg L-1。七个连续标准品预浓缩后构建的校准曲线在 0.3–800 μg L-1 的浓度范围内呈线性,相关系数为 0.9922。以相对标准偏差表示的日内和日间精密度分别为 1.4% 和 4.2%。实现了 490 的预浓缩因子,该方法用于分析加标废水。获得了 97.8% 至 102% 的令人满意的回收率。
更新日期:2019-07-02
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