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目的建立一种液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时检测饮用水中3种卤氧化物(高氯酸盐、氯酸盐及溴酸盐)的分析方法。方法水样直接经0.22μm水系滤膜过滤,采用100 mmol/L乙酸铵(A)和乙腈(B)作为流动相进行等度洗脱,经IC-Pak~(TM) Anion HR色谱柱分离,质谱(ESI-)采用多离子检测模式(MRM)对3种卤氧化物的定量离子和定性离子进行监测。结果本方法在6min内即完成3种目标化合物的分离分析。高氯酸盐及溴酸盐在0.5~50μg/L浓度范围内线性良好、氯酸盐在0.5~100μg/L浓度范围内线性良好(r≥0.999)。添加浓度为0.5、10.0、50.0μg/L,实验结果表明高氯酸盐、氯酸盐及溴酸盐的回收率可达84.8%~101.4%,相对标准偏差均小于10.0%(n=6)。高氯酸盐、氯酸盐及溴酸的检出限分别为0.1、0.2、0.2μg/L。结论该方法快速、准确、灵敏,适合测定饮用水中高氯酸盐、氯酸盐及溴酸盐的同时测定。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) for the simultaneous determination of three oxyhalides (perchlorate, chlorate and bromate) in drinking water method. Methods The water sample was directly filtered through 0.22 μm aqueous filter and wasocratically eluted with 100 mmol / L ammonium acetate (A) and acetonitrile (B) as the mobile phase. The fractions were separated on an IC-Pak ™ Anion HR column, Mass Spectrometry (ESI-) Multiple ion detection mode (MRM) was used to monitor the quantitative and qualitative ionization of three oxyhalides. Results The separation of the three target compounds was completed within 6 minutes. Perchlorate and bromate showed good linearity in the range of 0.5-50 μg / L, and chlorate was linear in the concentration range of 0.5-100 μg / L (r ≥ 0.999). The results showed that the recoveries of perchlorate, chlorate and bromate reached 84.8% -101.4% with relative standard deviations less than 10.0% (n = 6) . The detection limits of perchlorate, chlorate and bromate were 0.1, 0.2 and 0.2 μg / L respectively. Conclusion The method is rapid, accurate and sensitive and suitable for the simultaneous determination of perchlorate, chlorate and bromate in drinking water.