液相色谱-质谱测定水中高氯酸盐含量

Determination of perchlorate in water by liquid chromatography-mass spectrometry

目的建立水质中高氯酸盐的液相色谱/质谱联用测定方法,了解郑州自然水系中高氯酸盐的含量。方法选用Synergi TM Max-RP液相色谱分析柱,以高氯酸盐(Cl18O4-)为内标,进行UPLC/MS/MS测定。结果液相色谱/质谱联用方法测定高氯酸盐在2.0~200.0μg/L范围内具有良好的线性关系,检出限为0.50μg/L;在低、中、高3个添加水平下,回收率范围为81.7%~109.0%,相对标准偏差(RSD)为2.00%~4.78%。测定郑州市水中高氯酸盐含量,市政供水未超过10μg/L,地下水源水未超过15.0μg/L,均未超过国际标准(0.07mg/L),部分地表河流高达106.8μg/L。结论建立的方法操作简单、分离效果好、准确、灵敏度高,适用于水中高氯酸盐的分析测定,具有较好的应用价值;郑州市市政供水水质良好,地下水源水高氯酸盐含量有潜在风险,部分地表河流存在高氯酸盐污染风险,应引起重视,加强监管。

Objective To establish an analysis method for the determination of perchlorate in water by liquid chromatography-mass spectrometry(LC-MS);to understand the content of perchlorate in natural water supply in Zhengzhou.Methods The perchlorate was separated by Synergi TM Max-RP liquid chromatography separation column.Perchlorate(Cl18O4-)was used as internal standard to conduct detection by UPLC/MS/MS.Results There was a good linear relationship of perchlorate in the mass concentration range of 2.0-200.0μg/L.The detection limit was 0.50μg/L.The recovery rates were in the range of 81.7%-109% with the RSDs of 2.00%-4.78% at low,median and high spiked levels.The concentration of perchlorate was lower than 10.0μg/L for urban water supply and lower than 15.0μg/L for underground water supply and as high as 106.8μg/L for some surface river in Zhengzhou city,all satisfied the international standard(less than 0.07 mg/L).Conclusion The established method is simple,demonstrating good separation results,accurate and sensitive,which was suitable for the detection of perchlorate in water with a good practical application value.The quality of urban water supply in Zhengzhou city is good;the underground water haspotential risk while the surface river water has high risk of perchlorate pollution.Surveillance and management should be strengthened.