固相微萃取气相色谱法测定鱼胆中的五氯酚
Determination of Pentachlorophenol in Fish Gall Bladder by Solid Phase Microextraction Gas Chromatography
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摘要:
目的 研究运用自动固相微萃取(SPME)超声波辅助的萃取技术与气相色谱联用方法测定鱼胆汁中的五氯酚含量。 方法 优化鱼胆中五氯酚的顶空浓缩和微萃取技术,然后使用HP-5、DB-17 毛细管气相色谱法分离,电子捕获检测器定量测定。 结果 该方法线性范围为 0.08~100.00 μg/L,相关系数r=0.999 7,检出限为0.053 μg/L,加标回收率为81.5%~92.6%,相对标准偏差为3.6%~6.3%。 结论 固相微萃取气相色谱法简便、快速、灵敏,且无溶剂污染,是测定鱼胆中五氯酚含量的理想方法。 Abstract:Objective To establish determination methodology of pentachlorophenol in fish gall bladder by automatic solid-phase microextraction(SPME)with ancillary extraction of supersonic wave and gas chromatography. Methods Pentachlorophenol in fish gall bladder was extracted using optimized SPME technology, separated by HP-5 and DB-17 chromatographic columns and the content of pentachlorophenol in fish gall bladder was determined by electron capture detector(ECD)under optimized conditions. Results The linear range of the calibration curve was 0.08-100.00 μg/L with a correlation coefficient of 0.9997 and the detection limit for pentachlorophenol was 0.053 μg/L. The recovery rates were between 81.5%-92.6% and the relative standard deviations were between 3.6%-6.3%. Conclusion The method is simple, rapid and sensitive without solvent pollution, which is a ideal method for determination of pentachlorophenol in fish gall bladder.
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