关键词: 固相萃取, 固相微萃取, 气相色谱, 多溴联苯醚, 饮用水

Abstract: Objective: To establish a novel method for determining the contents of polybrominated diphenyl ethers (BDE-47 and BDE-99) in drinking water by solid phase extraction (SPE) or solid phase micro extraction (SPME) combined with gas chromatography (GC). Methods: In the SPE-GC method, 100 mL of water sample was purified by LC-C18 SPE column chromatography through elution with hexane. The eluent was evaporated to dryness in water bath at 80℃, and the remaining residue was re-dissolved with isooctane and made up to 1 mL. Finally, 1μL of the solution was injected into GC for the determination. The limits of detection (LOD) for BDE-47 and BDE-99 were 0.0008μg/L and 0.0009μg/L (RSN= 6), respectively, the regression equations showed good linearity with a correlation coefficient of 0.9996 and 0.9997, respectively, and the RSDs for 6 replicate determinations were in the range of 1.0%－4.9% and 0.96%－4.4%, respectively. In the SPME-GC method, 10 mL of water sample was placed into a 15-mL SPME bottle and adsorbed by solid-phase micro-extraction for 25 min at 40 ℃ with a rotation speed of 1150 r/min. Then, the fiber was air-dried, immediately followed by GC analysis. The LODs of the SPME-GC method for BDE-47 and BDE-99 were 0.0000μg/L and 0.0044μg/L (RSN = 6), respectively, the linear correlation coefficients were 0.9996 and 09992, respectively, and the RSDs for 6 replicate determinations varied in the range of 6.7%－11.4% and 6.0%－10.1%, respectively. Results: BDE-47 and BDE-99 were undetected in 52 samples randomly collected from a certain city. Conclusion: Both analytical methods are characterized by simplicity, rapidity, high precision, good accuracy and satisfactory recovery rate.

Key words: solid phase extraction, solid phase micro-extraction, gas chromatography, polybrominated diphenyl ethers, drinking water