Naing Nyi Nyi, Yau Li Sam Fong, Lee Hian Kee
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
J Chromatogr A. 2016 Apr 1;1440:23-30. doi: 10.1016/j.chroma.2016.02.046. Epub 2016 Feb 17.
A novel sorbent, magnetic chitosan functionalized graphene oxide (MCFG) was synthesized and used in the micro-solid-phase-extraction (μ-SPE) and gas chromatography-mass spectrometric (GC-MS) analysis of polycyclic aromatic hydrocarbons (PAHs) from water. Through the use of the magnetic sorbent, the μ-SPE device also functioned as a stir bar during extraction. Three types of MCFG were prepared using glutaraldehyde cross-linked chitosan and graphene oxide with different amounts of magnetic nanoparticles (Fe3O4) (0.05g, 0.07g and 0.1g). The material was characterized using Fourier transform infrared spectroscopy and field emission scanning electron microscopy. Parameters affecting the extraction such as the type of sorbent, extraction and desorption times, volume of sample solution and type of desorption solvent were optimized. Under the most favourable conditions, the highest extraction was obtained by using the composite prepared with 0.1g of Fe3O4. For the latter material as sorbent, the linearity of the analytes was in the range of 0.01 and 100μgL(-1) for naphthalene, fluoranthene and pyrene while acenaphthylene and phenanthrene exhibited linearity in the range of 0.05 and 100μgL(-1). For fluorene and anthracene, the linearity range was from 0.01 to 50μgL(-1). The coefficients of determination (r(2)) associated with the above linear ranges were higher than 0.987. The limits of detection from GC-MS analysis of the seven PAHs were in the range 0.2-1.8ngL(-1); limits of quantification were between 0.8 and 5.9ngL(-1) while the relative standard deviations (RSDs) varied from 2.1 to 8.2%. The recoveries of the method for the compounds at spiking levels of 1 and 5μgL(-1) were in the range 67.5-106.9% with RSDs below 15%. The enrichment factors were found to be in between 67 and 302. The developed method afforded an interesting and innovative approach using MCFG as an efficient and promising sorbent.
合成了一种新型吸附剂——磁性壳聚糖功能化氧化石墨烯(MCFG),并将其用于水中多环芳烃(PAHs)的微固相萃取(μ-SPE)和气相色谱-质谱联用(GC-MS)分析。通过使用磁性吸附剂,μ-SPE装置在萃取过程中还起到搅拌棒的作用。使用戊二醛交联壳聚糖和氧化石墨烯与不同量的磁性纳米颗粒(Fe3O4)(0.05g、0.07g和0.1g)制备了三种类型的MCFG。采用傅里叶变换红外光谱和场发射扫描电子显微镜对该材料进行了表征。对影响萃取的参数,如吸附剂类型、萃取和解吸时间、样品溶液体积和解吸溶剂类型进行了优化。在最有利的条件下,使用含0.1g Fe3O4制备的复合材料获得了最高的萃取效率。对于后一种材料作为吸附剂,萘、荧蒽和芘的分析物线性范围为0.01至100μg L(-1),而苊和菲的线性范围为0.05至100μg L(-1)。芴和蒽的线性范围为0.01至50μg L(-1)。与上述线性范围相关的测定系数(r(2))高于0.987。七种PAHs的GC-MS分析检测限在0.2-1.8ng L(-1)范围内;定量限在0.8至5.9ng L(-1)之间,而相对标准偏差(RSDs)在2.1%至8.2%之间变化。该方法在1和5μg L(-1)加标水平下对化合物的回收率在67.5-106.9%范围内,RSDs低于15%。富集因子在67至302之间。所开发的方法提供了一种有趣且创新的方法,使用MCFG作为一种高效且有前景的吸附剂。
J Chromatogr A. 2016-4-1
Materials (Basel). 2022-1-29