反相液相色谱/电喷雾质谱法分离水体中6种卤乙酸

Reverse Phase Liquid Chromatography/Electron Spray Ionization Mass Spectrometry for Separation of Haloacetic Acids in Drinking Water

建立了能够同时分离水体中6种卤乙酸的反相液相色谱—电喷雾质谱分析方法（RPLC-ESI-MS方法），确定了质谱优化条件（锥孔电压为15V，毛细管电压为4kV，脱溶剂气流量为400L／h，锥孔气流量为30L／h）。根据卤乙酸本身的强极性性质，采用乙腈和水作为流动相，同时在水相中投加25mmoL／L的醋酸铵缓冲盐，并用氨水调节水相pH值为9．7，以JJ50－2D型分析柱为分离柱，淋洗速度采用0．20mL／min，在最优质谱条件下直接进样，可使6种卤乙酸得到很好的分离。该检测方法的平均加标回收率为80％～102％，测定结果较为理想。

A specific method for the simultaneous analysis of the six haloacetic acids in water was established. The water samples were analyzed by reverse phase liquid chromatography/electron spray ionization mass spectrometry. The optimum MS conditions were determined as follows： cone voltage was 15 V, capillary voltage was 4 kV, desolvent gas flow was 400 L/h and cone gas flow 30 L/h. LC separation used JJS0-2D column. Eluates were acetonitrile and water containing 25 mmol/L ammonium acetate as buffering reagent. The water pH was adjusted to 9.7 with ammonia water. The elution velocity was 0.20 mL/min. Under such optimum conditions, the six haloacetic acids can be well separated. The average recovery rate is 80% to 102% , and the determined result is relatively ideal.