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

引用本文: 丘秀珍, 郭会时, 陈步青. 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[J]. 色谱, 2013, 31(8): 809-812. doi: 10.3724/SP.J.1123.2013.01029 shu

Citation: QIU Xiuzhen, GUO Huishi, CHEN Buqing. Determination of three phenolic compounds in water samples by solid phase extraction with microemulsion liquid chromatography[J]. Chinese Journal of Chromatography, 2013, 31(8): 809-812. doi: 10.3724/SP.J.1123.2013.01029 shu

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

通讯作者: 郭会时

基金项目:
教育部留学回国人员科研启动基金项目(第39批) (第39批)

广东省自然科学基金项目(9151200501000008) (9151200501000008)

韶关学院大学生创新创业立项项目.

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:

English

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

1.
College of Chemistry and Environmental Engineering, Shaoguan University, Shaoguan 512005, China

Corresponding author: 郭会时

Received Date: 14 January 2013
Fund Project:
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.

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:

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

1. [1] Zhou Y L. Journal of Environmental Monitoring Management and Technology (周艳玲. 环境监测管理与技术), 2011, 23(Suppl): 70[1] Zhou Y L. Journal of Environmental Monitoring Management and Technology (周艳玲. 环境监测管理与技术), 2011, 23(Suppl): 70
2. [2] Liu J F, Sun J, He Z G. Chinese Journal of Analytical Chemistry (刘建芳, 孙进, 何仲贵. 分析化学), 2007, 35(10): 1529[2] Liu J F, Sun J, He Z G. Chinese Journal of Analytical Chemistry (刘建芳, 孙进, 何仲贵. 分析化学), 2007, 35(10): 1529
3. [3] Zhang T, Cui Y. Chinese Journal of Chromatography (张婷, 崔颖. 色谱), 2011, 29(8): 768[3] Zhang T, Cui Y. Chinese Journal of Chromatography (张婷, 崔颖. 色谱), 2011, 29(8): 768
4. [4] Li N, Huang G L, Li Y L, et al. Chinese Journal of Analytical Chemistry (李宁, 黄光亮, 李玉兰, 等. 分析化学), 2009, 37(12): 1791[4] Li N, Huang G L, Li Y L, et al. Chinese Journal of Analytical Chemistry (李宁, 黄光亮, 李玉兰, 等. 分析化学), 2009, 37(12): 1791
5. [5] Li N, Hou X Z, Wang J X, et al. Journal of Instrumental Analysis (李宁, 侯璇珠, 王锦旋, 等. 分析测试学报), 2010, 29(2): 115[5] Li N, Hou X Z, Wang J X, et al. Journal of Instrumental Analysis (李宁, 侯璇珠, 王锦旋, 等. 分析测试学报), 2010, 29(2): 115
6. [6] Marsh A, Clark B J, Altria K D. Chromatographia, 2005, 61: 539 [6] Marsh A, Clark B J, Altria K D. Chromatographia, 2005, 61: 539
7. [7] Yang J R, Huang L N, Huang G L, et al. Chinese Journal of Chromatography (杨建锐, 黄丽娜, 黄光亮, 等. 色谱), 2011, 29(10): 995[7] Yang J R, Huang L N, Huang G L, et al. Chinese Journal of Chromatography (杨建锐, 黄丽娜, 黄光亮, 等. 色谱), 2011, 29(10): 995
8. [8] McEvoy E, Donegan S, Power J, et al. Chromatographia, 2008, 68: 49[8] McEvoy E, Donegan S, Power J, et al. Chromatographia, 2008, 68: 49
9. [9] He S, Zhang Z Y, Zhang S Y. Journal of Instrumental Analysis (贺帅, 张忠义, 张守尧. 分析测试学报), 2008, 27(6): 654[9] He S, Zhang Z Y, Zhang S Y. Journal of Instrumental Analysis (贺帅, 张忠义, 张守尧. 分析测试学报), 2008, 27(6): 654
10. [10] Chen L J, Zhang Z Y, Zhang S Y. Journal of Instrumental Analysis (陈莉婧, 张忠义, 张守尧. 分析测试学报), 2009, 28(10): 1217[10] Chen L J, Zhang Z Y, Zhang S Y. Journal of Instrumental Analysis (陈莉婧, 张忠义, 张守尧. 分析测试学报), 2009, 28(10): 1217
11. [11] Ren J B, Dai M, Li N. Journal of Instrumental Analysis (任晶波, 戴敏, 李宁. 分析测试学报), 2011, 30(5): 562[11] Ren J B, Dai M, Li N. Journal of Instrumental Analysis (任晶波, 戴敏, 李宁. 分析测试学报), 2011, 30(5): 562
12. [12] Altria K D, Marsh A, Clark B J. Chromatographia, 2006, 63: 309 [12] Altria K D, Marsh A, Clark B J. Chromatographia, 2006, 63: 309

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 392
HTML全文浏览量: 62

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 郭会时

English

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

Corresponding author: 郭会时

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 郭会时

English

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

Corresponding author: 郭会时

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs