高效液相色谱<b>-</b>串联质谱法同步测定饮用水中<b>18</b>种常见消毒副产物的方法研究

宁霄; 金绍明; 孙雯雯; 曹进; 裴宇盛

doi:10.19428/j.cnki.sjpm.2023.22731

高效液相色谱-串联质谱法同步测定饮用水中18种常见消毒副产物的方法研究

Simultaneous determination of 18 common disinfection by-product residues in drinking water by high performance liquid chromatography-tandem mass spectrometry

摘要

摘要:
目的基于超高效液相色谱-串联质谱（UHPLC⁃MS/MS）建立饮用水中18种常见卤氧化物和卤代乙酸消毒副产物的快速检测方法。
方法水样经0.22 μm亲水滤膜过滤后，采用PFP（2.1 mm× 100 mm，2.7 μm）五氟苯基色谱柱分离，0.1%乙酸和乙腈为流动相梯度洗脱，在阴离子电喷雾模式下电离，采用多反应监测（MRM）模式检测，外标法定量。
结果 4种卤氧化物和14种卤乙酸均在相应线性范围内，相关系数均>0.999。每种分析物1、10和20倍定量限浓度水平的平均加标回收率为91.6%~101.8%，相对标准偏差（RSD）为1.2%~6.4%。方法检出限和定量限分别为0.020~2 μg·L^-1和0.050~5 μg·L^-1。
结论此方法快速简便、灵敏度高、准确有效，可用于饮用水中18种常见消毒副产物的快速检测。

Abstract:
Objective A method was developed for the rapid determination of 18 common disinfection by-products including halogenated oxides and haloacetic acid （HAAs） in drinking water by high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS）.
Method The water sample was filtered by 0.22 μm hydrophilic membrane then the analytes were separated on a PFP （2.1 mm× 100 mm， 2.7 μm） pentafluorophenyl column with 0.1% acetic acid and acetonitrile as mobile phase gradient elution. Ionization in anionic electrospray mode was detected by multi-reaction monitoring （MRM） mode. The external standard method was used for quantitation.
Results The correlation coefficients of 18 disinfection by-products were above 0.999 in the corresponding linear range. The average spiked recoveries of 1， 10 and 20 times of LOQ of each analyte were 91.6%‒101.8%， and the relative standard deviation （RSD） was 1.2%‒6.4%. The LOD and LOQ were 0.020‒2 μg·L^-1 and 0.050‒5 μg·L^-1， respectively.
Conclusion This method is simple， sensitive and accurate， and could be used for the routine analysis of 18 common disinfection by-products in drinking water.

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