色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 809-812.DOI: 10.3724/SP.J.1123.2013.01029

• 技术与应用 • 上一篇    下一篇

固相萃取-微乳液相色谱法测定环境水体中的3种酚类化合物

丘秀珍, 郭会时, 陈步青   

  1. 韶关学院化学与环境工程学院, 广东 韶关 512005
  • 收稿日期:2013-01-14 修回日期:2013-03-22 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 郭会时
  • 基金资助:

    教育部留学回国人员科研启动基金项目(第39批);广东省自然科学基金项目(9151200501000008);韶关学院大学生创新创业立项项目.

Determination of three phenolic compounds in water samples by solid phase extraction with microemulsion liquid chromatography

QIU Xiuzhen, GUO Huishi, CHEN Buqing   

  1. College of Chemistry and Environmental Engineering, Shaoguan University, Shaoguan 512005, China
  • Received:2013-01-14 Revised:2013-03-22 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

PDF

196

被引次数

6

摘要：

建立了固相萃取-微乳液相色谱法同时测定环境水体中的苯酚、双酚A (BPA)、2,4-二氯苯酚3种酚类化合物的检测方法。水样加酸酸化后,经C18固相萃取小柱富集净化,用微乳液相色谱法测定3种目标物的含量。在Inertsil C18色谱柱(150 mm×4.6 mm, 5 μm)上以微乳(3.0%十二烷基硫酸钠(SDS)-6.0%正丁醇-0.8%正庚烷-90.2%(水+0.5%HAc))和乙腈作为流动相进行梯度洗脱,流速1.0 mL/min,检测波长280 nm。结果表明,苯酚、双酚A、2,4-二氯苯酚的检出限(S/N=3)依次为0.74、8.0、8.0 μg/L,线性范围在0.1~10 mg/L范围内,相关系数(r)均大于0.999。将3种酚类化合物定量加到空白水样中,苯酚、双酚A、2,4-二氯苯酚的加标回收率分别为82.7%、87.8%、82.6%,其RSD均小于5%(n=6)。对环境水样的酚类化合物分析也取得了良好的加标回收率,其值均在85.7%~113.2%之间。结果表明,该方法准确可靠、灵敏度高,适用于环境水体中酚类化合物的检测。

关键词: 2,4-二氯苯酚, 苯酚, 固相萃取, 双酚A, 微乳液相色谱

Abstract:

A method for the determination of phenol, bisphenol A (BPA), 2,4-dichlorophenol in water samples based on solid-phase extraction with microemulsion liquid chromatography(MELC) was established. The water sample was acidified, and then cleaned-up by a C18 solid-phase extraction cartridge. The separation was carried out on an Inertsil C18 (150 mm×4.6 mm, 5 μm) with a gradient elution using a microemulsion (consisting of 3.0% sodium dodecyl sulfate (SDS), 6.0% butyl alcohol, 0.8% n-heptane, 90.2% (water+0.5% acetic acid)) and acetonitrile as mobile phases at a flow rate of 1.0 mL/min and a detection wavelength of 280 nm. The detection limits (S/N=3) of phenol, BPA, 2,4-dichlorophenol were 0.74, 8.0, 8.0 μg/L, respectively. Good linearities were achieved for the target compounds over the range of 0.1-10 mg/L. The spiked recoveries of three phenolic compounds in blank water samples were 82.7%, 87.8%, 82.6% for phenol, BPA, 2,4-dichlorophenol respectively. The recoveries of target compounds in real water samples ranged from 85.7% to 113.2%. The developed method is simple, selective, sensitive and applicable for the analysis of environmental water samples.

Key words: 2,4-dichlorophenol, bisphenol A, microemulsion liquid chromatography (MELC), phenol, solid-phase extraction (SPE)

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