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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

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【作者】 金米聪马建明陈晓红李小平陈衡平

【Author】 Jin Mi-cong~1,Ma Jian-ming~2,Chen Xiao-hong~1,Li Xiao-ping~1,Chen Heng-ping~1(1.Ningbo Municipal Center for Disease Control and Prevention,Ningbo 315010,China;2.Cixi Municipal Center for Disease Control and Prevention,Cixi 315300,China)[HJ*2/5]

【机构】 浙江省宁波市疾病预防控制中心浙江省慈溪市疾病预防控制中心浙江省宁波市疾病预防控制中心 浙江宁波315010浙江慈溪315300浙江宁波315010

【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.

【基金】 宁波市医学科技计划资助项目(2002009,2003056)
  • 【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
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