Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran; Department of Chemistry, University of Waterloo, Ontario N2L 3G1 Waterloo, Canada.
J Chromatogr A. 2024 Aug 16;1730:465061. doi: 10.1016/j.chroma.2024.465061. Epub 2024 Jun 14.
In this research, electrospun nanofibers based on copper-based metal organic framework (MOF)/polyurethane (PU) were prepared in order to achieve an applicable and superior extractive phase. The incorporation of MOF, in the synthesized nanocomposite contributed to the enhanced sorption efficiency. The prepared sorbent was implemented for the thin film microextraction (TFME) of target compounds with subsequent quantification using gas chromatography-mass spectrometry (GC-MS). To obtain the maximum efficiency of the synthesized sorbent, the influential parameters on extraction and desorption steps, including the MOF percentage in nanocomposite, desorption solvent type and its volume, desorption time, solution ionic strength and extraction time were optimized. After method development, the linear dynamic range (0.02-700 μg L), limits of detection (LODs) (0.005-0.1 μg L) and limits of quantification (LOQs))0.02-0.33 μg L(were calculated. The relative standard deviations values for intra-day and inter-day analysis were found to be in the range of 4.3-5.3 % and 6.2-8.1 %, respectively. The developed method was validated for the TFME of model organochlorine (OC) pesticide residues in fish, soil and water samples. the recovery values for the spiked samples at two concentration levels of 5 and 100 µg l were found in the range of 72-110 %.
在这项研究中,制备了基于铜基金属有机骨架(MOF)/聚氨酯(PU)的静电纺纳米纤维,以获得一种适用且优越的萃取相。MOF 的掺入,在合成的纳米复合材料中,有助于提高吸附效率。制备的吸附剂用于目标化合物的薄膜微萃取(TFME),随后使用气相色谱-质谱联用(GC-MS)进行定量。为了获得合成吸附剂的最大效率,优化了萃取和洗脱步骤的影响参数,包括纳米复合材料中 MOF 的百分比、洗脱溶剂的类型及其体积、洗脱时间、溶液离子强度和萃取时间。方法开发后,计算了线性动态范围(0.02-700 μg L)、检测限(LODs)(0.005-0.1 μg L)和定量限(LOQs)(0.02-0.33 μg L)。日内和日间分析的相对标准偏差值分别在 4.3-5.3%和 6.2-8.1%的范围内。该方法已验证用于鱼类、土壤和水样中模型有机氯(OC)农药残留的 TFME。在 5 和 100 µg l 两个浓度水平下,加标样品的回收率在 72-110%的范围内。