摘要
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×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×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.
出处
《色谱》
CAS
CSCD
北大核心
2014年第5期535-538,共4页
Chinese Journal of Chromatography
基金
国家水体污染控制与治理重大专项(2009ZX07527-005)
宁波市自然科学基金项目(2011A610087
201201A6107004)
关键词
超高效液相色谱
亲水作用色谱
串联质谱
苦味酸
苦氨酸
ultra performance liquid chromatography (UPLC)
hydrophilic interaction liquidchromatography (HILIC)
tandem mass spectrometry (MS/MS)
picric acid
picramic acid