HPLC-MS-MS法与GC法对比测定饮用水中9种卤乙酸

Comparison of Ultra‑performance Liquid Chromatography Tandem Mass Spectrometry and Gas Chromatography for Determination of Nine Haloacetic Acids in Drinking Water

分别建立了采用气相色谱法与超高效液相-三重四极杆质谱法测定饮用水中9种卤乙酸的方法。采用气相色谱法测定时,水样经甲基叔丁基醚萃取后,采用HP-5色谱柱进行分离,ECD检测器检测。采用超高效液相-三重四极杆质谱法测定时,水样经PTFE滤膜过滤后直接上机测定,采用ACQUITY UPLC HSS■T3色谱柱进行分离,MRM负离子模式进行测定。两种方法的检出限均达到了μg/L级别,且回收率及精密度均满足检测要求。采用两种方法对质控样品进行独立样本t检验,测试结果无显著统计学差异;超高效液相-三重四极杆质谱法方法测定卤乙酸质控样品的测试结果更接近于已知质量浓度,且相比于气相色谱方法,其在前处理方法及时效性方面更具优势。

This paper established two methods of gas chromatography and ultra‑performance liquid chromatography tandem triple quadrupole mass spectrometry for the determination of 9 kinds of haloacetic acid in drinking water.In gas chromatography method,the water samples were extracted by methyl tert‑butyl ether,separated by HP-5 chromatographic column and detected by ECD detector.In ultra‑performance liquid chromatography tandem triple quadrupole mass spectrometry method,the water samples were filtered by PTFE filter,separated by ACQUITY UPLC HSS®T3 chromatographic column,and determined by MRM negative ion mode.The detection limits of the two methods reached the level ofμg/L,and the recovery rate and precision met the detection requirements.The two methods were used for independent sample t‑test of quality control samples,and the test results showed no significant statistical difference.The results of ultra‑performance liquid chromatography tandem triple quadrupole mass spectrometry for the determination of haloacetic acid quality control samples were closer to the known mass concentration.Compared with gas chromatography,it had more advantages in pre‑treatment method and timeliness.