单液滴微萃取/正相液相色谱法测定水中二氯酚和萘酚  

Determination of Dichlorophenol Isomers and Naphthol in Water by Single-drop Microextraction/Normal Phase Liquid Chromatography

作　　者：周建科[1] 宋歌[1] 刘瑞英[1] 张明翠[1] 

机构地区：[1]河北大学理化分析中心河北省分析科学技术重点实验室,河北保定071002

出　　处：《中国给水排水》2009年第8期76-79,共4页China Water & Wastewater

摘　　要：采用液下单液滴微萃取样品处理方法富集水中的2,6-二氯酚、2,4-二氯酚、3,4-二氯酚和α-萘酚,然后用高效液相色谱法测定。色谱条件为:Apollo Silica色谱柱(5μm,250mm×4.6 mmi.d.),柱温为室温,流速为1.0 mL/min,二氯甲烷、正己烷、甲醇(体积比为50∶50∶0.5)为流动相,在225 nm紫外波长下检测。最佳萃取条件:3μL四氯化碳液滴为萃取剂,30℃,转速为300 r/min,pH=4,NaCl含量为150 g/L,时间为10 min。2,4-二氯酚、2,6-二氯酚、3,4-二氯酚在0.001～25 mg/L范围内,α-萘酚在0.000 5～12.5 mg/L范围内线性良好,检出限为0.000 5～0.001 mg/L,加标回收率为75.3%～89.8%。A direct single-drop microextraction/high performance liquid chromatography （SDME- HPLC） method was used for the simultaneous determination of four phenols in water, including 2, 4-dichlorophenol, 2, 6-dichlorophenol, 3, 4-dichlorophenol, and α-naphthol. The chromatographic conditions are as follows ： Apollo Silica （5 μm, 250 × 4.6 mm i. d） is used ; The column temperature is room temperature; The flow rate is 1.0 mL/min; The mobil phase is dichloromethane/n-hexane/methanol （50 ： 50 ： 0.5 ） ; The wavelength of UV detector is 225 nm. The optimal extraction conditions are as follows ： The extraction solvent is 3 μL carbon tetrachloride; The extraction temperature is 30 ℃ ; The stirring rate is 300 r/min; The pH is 4; The sodium chloride concentration is 150 g/L; The extraction time is 10 min. The 2, 4-dichlorophenol, 2, 6-dichlorophenol, 3, 4-dichlorophenol have good linear correlation in a range of 0. 001 to 25 mg/L and the α-naphthol has good linear correlation in a range of 0. 000 5 to 12.5 mg/L. The detection limits of the four phenols are 0. 000 5 to 0. 001 mg/L. The average recovery is 75.3% to 89.8%.

关 键 词：二氯酚异构体 Α-萘酚 正相液相色谱 单液滴微萃取 

分 类 号：TU991.2[建筑科学—市政工程]