In this work, a laboratory preparation method based on sol–gel technology was proposed to develop a new kind of SPME (solid phase microextraction) fibers. Multi-walled carbon nanotubes (MWCNT) were selected as sol–gel active organic component. Stainless steel wires were used as the substrate of the fibers. Instead of traditional modification methods, microwave induced plasma was used to modify the stainless steel wire surface, resulting in a significant improvement in chemical adhesion of the fiber substrate and coating. The MWCNT coating exhibited several good properties. Acceptable fiber-to-fiber reproducibility (RSD ≤ 13%) and repeatability (RSD < 7%) were obtained. End-tidal breath of 10 normal humans were collected by Bio-VOC ® sampler and assayed by the optimized SPME-GC-MS method. The calibration curves were all linear ( R 2 ≥ 0.994) in the range from 0.03 to 403.3 ppbv for five alkanes. Detection limits (down to 0.001 ppbv) were about one order of magnitude better than those of commercial PDMS fibers. The recovery of the spiked alkanes in real breath sample at 1 ppbv ranged from 89.71 to 101.08% and the relative standard deviations were less than 8%. These results demonstrated the feasibility and practicality of the proposed preparation procedure. Applications of the in-house fabricated fibers for human breath analysis were successfully verified.
Shuaihua Zhang,Qian Yang,Zhi Li,Wenjin Wang,Xiaohuan Zang,Chun Wang,Zhi Wang
A hybrid composite featuring an iron-based metal-organic framework Material of Institute Lavoisier-88(Fe) and graphene oxide (MIL-88(Fe)/GO) was synthesized and used as the solid-phase microextraction (SPME) coating. The SPME fiber was prepared by covalent bonding of the MIL-88(Fe)/GO composite onto the stainless steel substrate. The fiber had a good durability and allowed >100 replicate extractions. The developed method, which combined the MIL-88(Fe)/GO coated fiber based SPME with gas chromatography-flame ionization detection (GC-FID), achieved low limits of detection (0.5–2.0 ng g −1 , S/N = 3) and good linearity ( r 2 > 0.994) for the phthalic acid esters (PAEs) from various vegetable oil samples. The repeatability and fiber-to-fiber reproducibility were in the range of 4.0–9.1% and 5.7–11.4%, respectively. The method was successfully applied to the analysis of PAEs from vegetable oil samples with good recoveries (83.1–104.1%) and satisfactory precisions (RSDs < 10.5%), indicating that the MIL-88(Fe)/GO hybrid composite is a good coating material for the SPME of PAEs.
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