Rozi Siti Khalijah Mahmad, Nodeh Hamid Rashidi, Kamboh Muhammad Afzal, Manan Ninie Suhana Abdul, Mohamad Sharifah
Department of Chemistry, Faculty of Science, University of Malaya.
School of Bioprocess Engineering, University of Malaysia Perlis.
J Oleo Sci. 2017 Jul 1;66(7):771-784. doi: 10.5650/jos.ess17016. Epub 2017 Jun 13.
A novel adsorbent, palm fatty acid coated magnetic FeO nanoparticles (MNP-FA) was successfully synthesized with immobilization of the palm fatty acid onto the surface of MNPs. The successful synthesis of MNP-FA was further confirmed by X-Ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Energy dispersive X-Ray spectroscopy (EDX) analyses and water contact angle (WCA) measurement. This newly synthesized MNP-FA was applied as magnetic solid phase extraction (MSPE) adsorbent for the enrichment of polycyclic aromatic hydrocarbons (PAHs), namely fluoranthene (FLT), pyrene (Pyr), chrysene (Cry) and benzo(a)pyrene (BaP) from environmental samples prior to High Performance Liquid Chromatography- Diode Array Detector (HPLC-DAD) analysis. The MSPE method was optimized by several parameters such as amount of sorbent, desorption solvent, volume of desorption solvent, extraction time, desorption time, pH and sample volume. Under the optimized conditions, MSPE method provided a low detection limit (LOD) for FLT, Pyr, Cry and BaP in the range of 0.01-0.05 ng mL. The PAHs recoveries of the spiked leachate samples ranged from 98.5% to 113.8% with the RSDs (n = 5) ranging from 3.5% to 12.2%, while for the spiked sludge samples, the recoveries ranged from 81.1% to 119.3% with the RSDs (n = 5) ranging from 3.1% to 13.6%. The recyclability study revealed that MNP-FA has excellent reusability up to five times. Chromatrographic analysis demonstrated the suitability of MNP-FA as MSPE adsorbent for the efficient extraction of PAHs from environmental samples.
一种新型吸附剂——棕榈脂肪酸包覆磁性FeO纳米颗粒(MNP-FA)已成功合成,即将棕榈脂肪酸固定在MNPs表面。通过X射线衍射(XRD)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、能量色散X射线光谱(EDX)分析以及水接触角(WCA)测量,进一步证实了MNP-FA的成功合成。这种新合成的MNP-FA被用作磁性固相萃取(MSPE)吸附剂,用于在高效液相色谱-二极管阵列检测器(HPLC-DAD)分析之前,从环境样品中富集多环芳烃(PAHs),即荧蒽(FLT)、芘(Pyr)、 Chrysene(Cry)和苯并[a]芘(BaP)。通过吸附剂用量、解吸溶剂、解吸溶剂体积、萃取时间、解吸时间、pH值和样品体积等几个参数对MSPE方法进行了优化。在优化条件下,MSPE方法对FLT、Pyr、Cry和BaP的检测限(LOD)在0.01-0.05 ng/mL范围内。加标渗滤液样品中PAHs的回收率在98.5%至113.8%之间,相对标准偏差(RSD,n = 5)在3.5%至12.2%之间;而加标污泥样品的回收率在81.1%至119.3%之间,RSD(n = 5)在3.1%至13.6%之间。可回收性研究表明,MNP-FA具有高达五次的优异可重复使用性。色谱分析表明,MNP-FA作为MSPE吸附剂适用于从环境样品中高效萃取PAHs。