液相色谱-串联质谱法测定饮用水中的卤氧化物

Determination of oxyhalides in drinking water by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  卤氧化物  高氯酸盐  氯酸盐  溴酸盐

英文关键词:liquid chromatography-tandem mass spectrometry  oxyhalides  perchlorate  chlorate  bromate

中文摘要:

      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0.22 μm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-PakTM 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6 min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0.5~50 μg/L浓度范围内线性良好、氯酸盐在0.5~100 μg/L浓度范围内线性良好(r≥0.999)。添加浓度为0.5、10.0、50.0 μg/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、0.2 μg/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。

英文摘要:

      Objective To establish a method for the simultaneous determination of 3 kinds of oxyhalides (perchlorate, chlorate and bromate) in drinking water by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Water samples were directly filtered with 0.22 μm hydrophilic filter membrane, and then the 3 kinds of oxyhalides in the water samples were separated on an IC-PakTM Anion HR column using an isocratic elution program of 100 mmol/L ammonium acetate solution (A) and acetonitrile (B). Using LC-MS/MS (ESI-) with multiple reactions monitoring (MRM), identification of the 3 kinds of oxyhalides was performed based upon the intensities of fragments. Results The 3 kinds of oxyhalides were separated and detected within 6 min. Perchlorate and bromate had good linear relationships in the range of 0.5~50 μg/L, and chlorate in the range of 0.5~100 μg/L (r≥0.999). The recoveries were ranged from 84.8% to 101.4% for the 3 kinds of oxyhalides with 3 spiked levels of 0.5, 10, 50 μg/L. The relative standard deviations (RSDs) were less than 10.0% (n=6), and the limits of detection for perchlorate, chlorate and bromate were 0.1, 0.2, 0.2 μg/L, respectively. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for the simultaneous determination of perchlorate, chlorate and bromated in drinking water.