色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 535-538.DOI: 10.3724/SP.J.1123.2013.11037

• 技术与应用 • 上一篇    下一篇

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

钱飞中1, 朱丽波1, 徐能斌1, 冯加永1, 洪正昉2, 徐立红3, 陈钟佺1, 汪晟乐1   

  1. 1. 宁波市环境监测中心, 浙江 宁波 315012;
    2. 浙江省环境监测中心, 浙江 杭州 310012;
    3. 绍兴市环境监测中心, 浙江 绍兴 312000
  • 收稿日期:2013-11-19 修回日期:2014-02-19 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 冯加永
  • 基金资助:

    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）.

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

QIAN Feizhong1, ZHU Libo1, XU Nengbin1, FENG Jiayong1, HONG Zhengfang2, XU Lihong3, CHEN Zhongquan1, WANG Shengle1   

  1. 1. Ningbo Environmental Monitoring Center, Ningbo 315012, China;
    2. Zhejiang Environmental Monitoring Center, Hangzhou 310012, China;
    3. Shaoxing Environmental Monitoring Center, Shaoxing 312000, China
  • Received:2013-11-19 Revised:2014-02-19 Online:2014-05-08 Published:2014-04-26

PDF

215

被引次数

18

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 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。

关键词: 超高效液相色谱, 串联质谱, 苦氨酸, 苦味酸, 亲水作用色谱

Abstract:

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.

Key words: hydrophilic interaction liquid chromatography (HILIC), picramic acid, picric acid, tandem mass spectrometry (MS/MS), ultra performance liquid chromatography (UPLC)

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