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

摘要

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(1.7 μm×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 ～ 100 μg/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 ～0.66 μg/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 the determination of dichloroaetic acid and trichloroacetic acid in water.Multiple reaction monitoring (MRM) with negative electrospray ionization(ESI-) in MS/MS was used for quantification.After being filtering through PVDF needle filter,the sample was separated on a ACQUITY CSH column with the mobile phases of acetonitrile and 0.05％ (V/V) acetic acid aqueous solution with gradient elution mode.The results displayed that two compounds showed good linearities ranging from 2.0 μg/L to 100 iμg/L.The linear correlation coefficients were 0.9992 ～ 0.9997.The limits of detection were 0.41 ～ 0.66μg/L.The recovery rates of the three levels of high,medium and low were 96.4％ ～ 113.0％.The relative standard deviations (RSDs) range were 0.81％ ～2.62％.The method wasrapid,convenient,had high sensitivity and good reproducibility.It could be used for rapid detection of dichloroacetic acid and trichloroacetic acid in tap water.