超高效亲水作用色谱-串联质谱法检测水中的苦味酸及苦氨酸

Analysis of picric acid and picramic acid in water samples by ultra performance hydrophilic interaction chromatography-tandem mass spectrometry

建立了一种超高效亲水作用色谱-串联质谱检测水中苦味酸及其降解产物苦氨酸的方法。采用 Acquity UP-LC BEH HILIC亲水作用色谱柱（100 mm＆#215;2.1 mm，1.7μm，Waters）分离，用电喷雾电离串联质谱检测。地表水样品经过0.2μm滤膜过滤之后即可直接进样，加标回收率达89％~107％；废水样品通过固相萃取（ SPE）净化后进样分析，加标回收率达72％~101％。方法重复性的相对标准偏差为4.9％~14.7％。本方法对苦味酸和苦氨酸的检出限分别为0.1μg/L和0.3μg/L。此方法快速、准确，特异性强，灵敏度高，样品前处理方法简便易行，适用于地表水、废水样品的检测。

An ultra performance liquid chromatography/tandem mass spectrometry（ UPLC-MS/MS）method was developed for the determination of picric acid and its reductive transformation product picramic acid in aqueous samples. A hydrophilic interaction liquid chromatography （HILIC）column（Acquity UPLC BEH HILIC;100 mm＆#215;2. 1 mm,1. 7 μm）was used for the sep-aration. Surface water samples could be injected into the UPLC system just after being filtered through a 0. 2 μm membrane. The satisfactory recoveries of picric acid and picramic acid were in the range of 89%-107%. Waste water samples were purified by solid phase extraction（ SPE）, and then were analyzed. The recoveries of picric acid and picramic acid in waste water were 72%-101%. The reproducibility of the method was good with the RSDs of 4. 9%-14. 7%. The limits of detection（ LODs）of picric acid and picramic acid were 0. 1 μg/L and 0. 3 μg/L,re-spectively. This proposed method is rapid,highly specific and suitable for the confirmation and quantitative determination of picric acid and picramic acid in surface water and waste water.