Determination of Haloacetic Acids in Drinking Water Using Ultra Performance Liquid Chromatography Coupled with Solid phase Extraction[J]. 2011,30(3):248-253.
Determination of Haloacetic Acids in Drinking Water Using Ultra Performance Liquid Chromatography Coupled with Solid phase Extraction[J]. 2011,30(3):248-253.DOI:
建立了固相萃取/超高效液相色谱(SPE/UPLC)测定饮用水中9种痕量卤乙酸(HAAs)的分析方法。对固相萃取和液相色谱等分析条件进行了优化,选择Lichrolut EN 固相萃取小柱富集饮用水中的HAAs,三乙胺-磷酸缓冲液和甲醇作为UPLC的流动相。在优化的分析条件下,9种卤乙酸在6 min内实现基线分离,所有目标物在一定质量浓度范围内线性良好,相关系数为0.995 7~0.999 9;一氯乙酸(MCAA)的检出限为10.85 μg/L,其它8种化合物的检出限为0.25~0.70 μg/L;除MCAA外,其它目标物在低、中、高3种加标水平的回收率为60%~106%。方法的相对标准偏差(RSD,n=5)为2.0%~5.7%。将此方法应用于我国北方某城市自来水中卤乙酸的测定,5种HAAs被检出。方法灵敏度高、简便快捷,可用于生活饮用水中痕量卤乙酸的测定。
Abstract
An ultra performance liquid chromatography(UPLC)coupled with solid phase extraction(SPE) method was established for the determination of nine haloacetic acids(HAAs) in drinking water. The experimental conditions of UPLC and SPE were optimized. Three SPE cartridges with different sorbents were tested,and Lichrolut EN cartridges showed the best recoveries. A good baseline separation of target compounds were obtained in 6 minutes when using methanol and triethylamine phosphate buffer(pH 5.0) as mobile phase,triethylamine as ion pair reagent. The calibration curves of nine HAAs were linear in the certain concentration range with correlation coefficients of 0.995 7 -0.999 9. The limit of detection(LOD,S/N≥3) for monochloroacetic acid(MCAA) was 10.85 μg/L,and those for rest of target compounds were between 0.25 μg/L and 070 μg/L. Recoveries of HAAs at three spiked concentration levels ranged from 60% to 106% except for MCAA. The relative standard deviations(RSDs,n=5) of the method were between 2.0% and 5.7%. This method was applied in the determination of HAAs in tap water samples from a northern city in China,and five HAAs were detected.Therefore,the method was sensitive and convenient,and could be used in the trace determination of HAAs in drinking water.
关键词
卤乙酸固相萃取离子对超高效液相色谱饮用水
Keywords
haloacetic acidssolid phase extractionion pairultra performance liquid chromatographydrinking water