超高效液相色谱-串联质谱法检测饮用水中二氯乙酸和三氯乙酸

Determination of Dichloroacetic Acid and Trichloroacetic Acid in Drinking Water by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)

建立了超高效液相色谱-串联质谱法分析饮用水中二氯乙酸、三氯乙酸的分析方法。样品经PVDF针式过滤器后,采用ACQUITY CSH色谱柱(1.7μm×2.1 mm×50 mm),0.05%乙酸水和乙腈作为流动相进行梯度洗脱,质谱采用电喷雾负离子电离,多反应监测模式(MRM)检测。试验表明:二种卤乙酸在2.0～100μg/L线性关系良好,相关系数为0.999 2～0.999 7,方法的检出限为0.41～0.66μg/L;高、中、低三个添加水平的回收率为96.4%～113.0%,相对标准偏差为0.81%～2.62%。该方法灵敏,准确且重现性好,分析速度快,是一种适于实际水样中二氯乙酸、三氯乙酸检测分析的方法。

An ultra performance liquid chromatography-tandem mass spectrometry （ UPLC-MS/MS ） was developed for thedetermination of dichloroaetic acid and trichloroacetic acid in water. Multiple reaction monitoring （ MRM） with negative electro sprayionizat ion（ ESI ） in MS/MS was used for quantification. After being filtering through PVDF needle f i lter,the sample was separated ona ACQUITY CSH column with the mobile phases of acetonitrile and 0 . 05% （ V/V） acetic acid aqueous solution with gradient elutionmode. The results displayed that two compounds showed good l inearities ranging from 2. 0 jjig/L to 100 jjig/L. The linear correlationcoef f icients were 0.9992 - 0. 9997. The limits of detection were 0. 41 -0 . 6 6 jjig/L. The recovery rates of the three lev e ls of h ig h,medium and low were 96. 4% ？1 1 3 . 0% . The relative standard deviations （ R SD s ） range were 0 . 81% -2 . 6 2% . The method wasrap id , con v en ien t , had high sensitivity and good reproducibility. Itcould be used for rapid detection of dichloroacetic acid andrichloroacetic acid in tap water.