摘要
A one-pot PEG-modified MIL-88B(Fe) coating was developed for breath aldehydes. • The 10% PEG/Fe³⁺ ratio gave the highest responses for all five aldehydes. • Detection limits were 0.018–0.030 ng mL⁻¹ with precision below 10%. • The coating retained 87.9–93.9% response after 110 extraction cycles. A polyethylene glycol (PEG)-modified MIL-88B(Fe) composite was synthesized by a one-pot route and evaluated as a coating for headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC–MS) for the determination of five C6–C10 aldehydes. Among the materials prepared at PEG/Fe 3+ molar ratios of 0, 5, 10, and 15%, PEG 10 @MIL-88B(Fe) produced the highest peak areas for all five aldehydes. Characterization by powder X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, and N 2 adsorption–desorption analysis supported PEG modification while retaining the structural characteristics of MIL-88B(Fe). Under the optimized conditions, the developed method provided enrichment factors of 2563–15,562. Calibration curves were linear over 0.1–500 ng mL –1 (R 2 = 0.9911–0.9988), with LODs of 0.018–0.030 and LOQs of 0.059–0.099 ng mL –1 of calibration solution (liquid-standard-equivalent). Intra-day, inter-day, fiber-to-fiber, and batch-to-batch RSDs were 3.9–5.9%, 4.2–8.2%, 4.0–9.8%, and 5.3–10.1%, respectively. The method showed limited interference from representative breath volatile organic compounds, with relative responses of 89.30–92.02%, while matrix effects ranged from 94.7% to 104.1%. After 110 extraction/desorption cycles, the coating retained 87.9–93.9% of its initial response. The PEG 10 @MIL-88B(Fe)-coated SPME fiber was applied to exhaled-breath samples, with spike recoveries of 87.2–105.5%, supporting its applicability to the trace determination of C6–C10 aldehydes in exhaled breath. Download: Download high-res image (309KB) Download: Download full-size image
危险品化学品经营许可证（带存储）