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饮用水中3种一氯酚异构体的液相色谱-质谱联用法测定研究
Simultaneous determination of 3 trace monochlorophenols in water by high-performance liquid chromatography mass spectrometry
【摘要】 目的:建立一种能同时测定饮用水中2-氯酚、3-氯酚和4-氯酚的检测方法。方法:水样经Oasis(HLB固相萃取小柱富集、净化后,在C8柱(250 mm×4.0 mm×5μm)上,以乙酸-乙酸铵缓冲溶液(5 mmol/L,pH=4.5)/乙腈/甲醇(65:28:7)为流动相,采用大气压化学电离(APC I)离子化方式在选择离子监测(SIM)模式下进行检测,定量检测离子为m/:z 127[M-H]-。结果:2-氯酚、3-氯酚和4-氯酚的日内与日间精密度分别小于9.3%和10.9%,它们在0.05~5.00μg/L范围均具有良好的线性,水样中它们的最低定量检出限分别为0.05、0.02和0.02μg/L。结论:本方法可用于饮用水中痕量一氯酚的测定。
【Abstract】 Objective:To develop a novel,sensitive and accurate method for the simultaneous determination of 3 monochlorophenols(MCP) in drinking water samples by high-performance liquid chromatography(HPLC) coupled with an atmospheric pressure chemical ionization mass spectrometry(APCI-MS).Methods:Drinking water was preconcentrated by solid-phase extraction(SPE).The HPLC separation was carried out with a carbamate analysis C8 column(250 mm×4.0 mm×5 μm) using acetic acid-acetic acid ammonium(5 mmol/L,pH=4.5)/acetonitrile/methanol(65:28:7) as mobile phase in isocratic mode at a constant flow rate of 1.0 ml/min.Detection was performed by an APCI-MS in the negative mode.The molecular ion m/z 127 \-was selected for the quantification in selected ion monitoring(SIM) mode.Results:Within-day and day-to-day relative standard deviations were less than 9.3% and 10.9%,respectively.The linear range was 0.055.00 μg/L for each MCP.The limits of quantification(LOQs) in water samples were 0.05,0.02 and 0.02 μg/L for 2-MCP,3-MCP and 4-MCP,respectively.Conclusion:The method allows the 3 target compounds in water samples to be determined at the μg/L levels,and it has been successfully applied to the routine analyses.
【Key words】 HPLC-MS; 2-Chlorophenol; 3-Chlorophenol; 4-Chlorophenol; Drinking water;
- 【文献出处】 中国卫生检验杂志 ,Chinese Journal of Health Laboratory Technology , 编辑部邮箱 ,2006年05期
- 【分类号】R123.1
- 【被引频次】31
- 【下载频次】267