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目的探讨顶空固相微萃取(SPME)技术与气相色谱法联用测定水中五氯酚。方法优化水中五氯酚的SPME顶空浓缩和微萃取技术,然后使用毛细气相色谱法分离,电子捕获检测器定量测定。结果水样调pH=2,60℃搅拌平衡40min,聚丙烯酸酯萃取头(85μm)顶空吸附10min,280℃解吸3min。最低检出浓度为0.13μg/L;五氯酚线性范围0～12μg/L,r=0.999;对水加标五氯酚1、6、10μg/L回收率分别为88.9%～105.0%、88.9%～102.8%和98.0%～99.5%,相对标准偏差分别为4.9%～8.4%、3.1%～8.5%和4.0%～5.4%(n=6)。结论该方法简便、灵敏、稳定,且无溶剂污染,是测定水中五氯酚理想的方法。
Objective To investigate the determination of pentachlorophenol in water by headspace solid phase microextraction (SPME) coupled with gas chromatography. Methods Optimization of SPME headspace concentration and microextraction of pentachlorophenol in water was performed, then separated by capillary gas chromatography and quantified by electron capture detector. Results The water sample was adjusted to pH 2 and stirred at 60 ℃ for 40 min. The heads of polyacrylate extraction heads (85 μm) were adsorbed for 10 min and desorbed at 280 ° C for 3 min. The minimum detectable concentration was 0.13μg / L and the linear range of pentachlorophenol was 0-12μg / L, r = 0.999. The recoveries of water-spiked with pentachlorophenol at 1, 6 and 10μg / L were 88.9% -105.0% and 88.9% % ~ 102.8% and 98.0% ~ 99.5%, respectively. The relative standard deviations were 4.9% -8.4%, 3.1% -8.5% and 4.0% -5.4%, respectively (n = 6). Conclusion The method is simple, sensitive, stable and solvent-free. It is an ideal method for the determination of pentachlorophenol in water.