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

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 UPLC BEH HILIC亲水作用色谱柱（100 mm×2.1 mm，1.7 μm，Waters）分离，用电喷雾电离串联质谱检测。地表水样品经过0.2 μm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0.1 μg/L和0.3 μg/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。

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

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×2.1 mm, 1.7 μm) was used for the separation. 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, respectively. 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.