Su Shaowei, Chen Beibei, He Man, Hu Bin
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Talanta. 2014 Jun;123:1-9. doi: 10.1016/j.talanta.2014.01.061. Epub 2014 Jan 31.
In this work, a novel graphene oxide-silica (GO-silica) composite coating was prepared for hollow fiber solid phase microextraction (HF-SPME) of trace Mn, Co, Ni, Cu, Cd and Pb followed by on-line inductively coupled plasma mass spectrometry (ICP-MS) detection. The structure of the prepared graphene oxide and GO-silica composite was studied and elucidated by atomic force microscopy (AFM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The GO-silica composite coated hollow fiber was characterized by scanning electron microscope (SEM), and the results show that the GO-silica composite coating possessed a homogeneous and wrinkled structure. Various experimental parameters affecting the extraction of the target metal ions by GO-silica composite coated HF-SPME have been investigated carefully. Under the optimum conditions, the limits of detection (LODs, 3σ) for Mn, Co, Ni, Cu, Cd and Pb were 7.5, 0.39, 20, 23, 6.7 and 28 ng L(-1) and the relative standard deviations (RSDs, c(Mn, Co, Cd)=0.05 μg L(-1), c(Ni, Cu, Pb)=0.2 μg L(-1), n=7) were 7.2, 7.0, 5.6, 7.3, 7.8 and 4.6%, respectively. The accuracy of the proposed method was validated by the analysis of Certified Reference Material of GSBZ 50009-88 environmental water and the determined values were in a good agreement with the certified values. The proposed method has been successfully applied for the determination of trace metals in real environmental water samples with recoveries ranging from 85 to 119%.
在本工作中，制备了一种新型的氧化石墨烯-二氧化硅（GO-二氧化硅）复合涂层，用于痕量锰、钴、镍、铜、镉和铅的中空纤维固相微萃取（HF-SPME），随后进行在线电感耦合等离子体质谱（ICP-MS）检测。通过原子力显微镜（AFM）、透射电子显微镜（TEM）、傅里叶变换红外光谱（FT-IR）和X射线光电子能谱（XPS）对制备的氧化石墨烯和GO-二氧化硅复合材料的结构进行了研究和阐释。用扫描电子显微镜（SEM）对GO-二氧化硅复合涂层中空纤维进行了表征，结果表明GO-二氧化硅复合涂层具有均匀且有褶皱的结构。仔细研究了影响GO-二氧化硅复合涂层HF-SPME萃取目标金属离子的各种实验参数。在最佳条件下，锰、钴、镍、铜、镉和铅的检测限（LODs，3σ）分别为7.5、0.39、20、23、6.7和28 ng L⁻¹，相对标准偏差（RSDs，c（锰、钴、镉）=0.05 μg L⁻¹，c（镍、铜、铅）=0.2 μg L⁻¹，n = 7）分别为7.2%、7.0%、5.6%、7.3%、7.8%和4.6%。通过分析GSBZ 50009-88环境水标准物质验证了该方法的准确性，测定值与认定值吻合良好。该方法已成功应用于实际环境水样中痕量金属的测定，回收率在85%至119%之间。
