Ma Mingguang, Wei Yunxia, Liu Fang
College of Chemistry and Chemical Engineering, Lanzhou City University Lanzhou 730070 China
RSC Adv. 2021 Nov 4;11(57):35842-35853. doi: 10.1039/d1ra05966a.
Immobilized TiO nanoparticles modified by nanoscale CuS (CuS@TiONPs) were successfully synthesized and used as fibers for solid-phase microextraction (SPME) for the determination of some polycyclic aromatic hydrocarbons (PAHs) in water samples. A novel fiber has been developed by postprecipitation of CuS coated the titania nanoparticles grown on a titanium wire annealed at 550 °C in a nitrogen ambient atmosphere. Its morphology and surface properties were characterized by scanning electron microscopy and energy dispersive X-ray spectrometry. It was connected to high performance liquid chromatography-ultraviolet detector (HPLC-UV) equipment by replacing the sample loop of a six-port injection valve, building the online SPME-HPLC-UV system. Variables affecting extraction procedures, including desorption time, stirring speed, extraction temperature, extraction time and ionic strength were investigated and the parameters were optimized. The SPME fiber exhibits high selectivity for the five PAHs studied. The linear ranges varied between 0.15 μg L and 200 μg L with correlation coefficients ranging from 0.9913 to 0.9985. LODs and LOQs ranged from 0.02-0.04 μg L and 0.07-0.13 μg L. RSDs for one fiber and fiber-to-fiber were in the range of 3.2-4.3% and 4.6-6.8%, respectively. Additionally, the fiber possessed advantages such as resistance to organic solvent, high mechanical strength and difficult breakage, making it have strong potential applications in the selective extraction of PAHs from complex water samples at trace levels.
成功合成了由纳米级硫化铜修饰的固定化二氧化钛纳米颗粒(CuS@TiONPs),并将其用作固相微萃取(SPME)纤维,用于测定水样中的某些多环芳烃(PAHs)。通过在氮气环境气氛中于550℃退火的钛丝上生长的二氧化钛纳米颗粒上后沉淀硫化铜,开发了一种新型纤维。通过扫描电子显微镜和能量色散X射线光谱对其形态和表面性质进行了表征。通过更换六通进样阀的样品环,将其连接到高效液相色谱-紫外检测器(HPLC-UV)设备上,构建了在线SPME-HPLC-UV系统。研究了影响萃取过程的变量,包括解吸时间、搅拌速度、萃取温度、萃取时间和离子强度,并对参数进行了优化。该SPME纤维对所研究的五种多环芳烃表现出高选择性。线性范围在0.15 μg/L至200 μg/L之间,相关系数在0.9913至0.9985之间。检测限和定量限分别为0.02 - 0.04 μg/L和0.07 - 0.13 μg/L。一根纤维和不同纤维之间的相对标准偏差分别在3.2 - 4.3%和4.6 - 6.8%范围内。此外,该纤维具有耐有机溶剂、机械强度高和不易断裂等优点,使其在从复杂水样中痕量选择性萃取多环芳烃方面具有很强的潜在应用价值。