Analysis of BTEX compounds by combined hollow fiber dispersive liquid-liquid microextraction and solid-phase microextraction with GC-FID detection
摘要
A novel analytical method combining hollow fiber (HF) dispersive liquid-liquid microextraction (DLLME) with solid-phase microextraction (SPME) followed by gas chromatography-flame ionization detection (GC-FID) was developed for the trace determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water samples. The sequential approach uses DLLME for high enrichment and HF-SPME for matrix cleanup and direct thermal desorption. Under optimized conditions (extraction solvent: 35 µL chloroform; dispersive solvent: 300 µL methanol; HF length: 1.5 cm; no salt; ambient temperature), the method achieved ultra-low detection limits (0.03–0.45 ng/L), which are substantially below regulatory limits (e.g., EPA MCL of 500 ng/L for benzene). The linear range spanned six orders of magnitude (0.0001–1000 µg/L) using segmented calibration. Accuracy was good (RSD: 2.3–5.1% intra-day; inter-day RSD: 4.2–7.8% ), and recoveries from spiked natural water samples (tap, well, river, spring, and wastewater) ranged from 88 to 110%. The method is green, using only 35 µL of organic solvent per extraction, and requires only 7 min extraction time. This technique is more sensitive and has a greater dynamic range than conventional methods such as HF-LPME, HS-SPME, and DLLME.