超声辅助-原位生成离子液体分散液液微萃取结合高效液相色谱法测定水样中的莠去津

潘闽君; 曹茜; 景明; 李晋阳; 陈家玮

doi:10.15898/j.cnki.11-2131/td.2015.03.016

超声辅助-原位生成离子液体分散液液微萃取结合高效液相色谱法测定水样中的莠去津

1.
生物地质与环境地质国家重点实验室, 北京 100083

2.
中国地质大学(北京)地球科学与资源学院, 北京 100083

基金项目: 国家自然科学基金面上项目(41272061, 41472232);生物地质与环境地质国家重点实验室开放基金(GBL21404);中央高校基本科研业务费优秀教师项目; 国家大学生创新实验计划项目

详细信息

作者简介: 潘闽君, 地质学专业. E-mail: panminjun1107@hotmail.com.

通讯作者: 陈家玮, 教授, 博士生导师, 从事环境地球化学研究. E-mail: chenjiawei@cugb.edu.cn.

中图分类号: S482.32;O658.2;O657.63

收稿日期: 2014-08-07

修回日期: 2015-05-12

录用日期: 2015-05-20

刊出日期: 2015-03-25

HPLC Determination of Atrazine in Water Using Dispersive Liquid-Liquid Microextraction Based on Ultrasonic-assisted in situ Ionic Liquid Formation

1.
State Key Laboratory of Biogeology and Environmental Geology, Beijing 100083, China

2.
School of Earth Sciences and Resources, China University of Geosciences, Beijing 100083, China

More Information

Corresponding author: CHEN Jia-wei, chenjiawei@cugb.edu.cn

Received Date: 07 August 2014

Revised Date: 12 May 2015

Accepted Date: 20 May 2015

Publish Date: 25 March 2015

摘要

摘要:
本文引入绿色溶剂离子液体作为萃取剂, 建立了超声辅助-原位生成离子液体分散液液微萃取水样中莠去津的方法。即处理5 mL水溶液样品, 以80 μL的[HMIM]Cl为萃取剂, 加入400 μL配对离子交换剂双三氟甲磺酰亚胺锂盐(LiNTf₂), 通过原位生成的疏水性离子液体[HMIM]NTf₂, 对水中莠去津进行液液微萃取, 经辅助超声10 min后4000 r/min离心8 min, 结合高效液相色谱测定莠去津。莠去津的检出限为0.01 mg/L, 方法线性范围为0.01~0.5 mg/L, 加标回收率(100.4%~106.7%)显著优于直接离子液体分散液液萃取法( < 67%)。这种原位生成离子液体微萃取技术有望应用于更广泛的有机污染物分析检测中。
- 莠去津 /
- 原位生成离子液体 /
- 分散液液微萃取 /
- 高效液相色谱法
Abstract:
A kind of green solvent, ionic liquid, was introduced as an extracting agent, and a new method of dispersive liquid-liquid microextraction based on ultrasonic-assisted in situ ionic liquid formation (DLLM-UAISLF) was established for the High Performance Liquid Chromatography (HPLC) determination of atrazine in water. Five mL of water was treated using 80 μL of [HMim]Cl as the extracting agent, 400 μL of LiNTf₂ as the ion-exchange material, ultrasound time of 10 minutes and centrifuge time of 8 minutes at 4000 r/min. During this process, the droplets of ionic liquid [HMim]NTf₂ were formed in water and the precipitates were then separated for determination of atrazine by HPLC. The detection limit of atrazine is 0.01 mg/L and the detection values range from 0.01 to 0.5 mg/L. The proposed method yielded recoveries of 100.4%-106.7%, which are obviously better than those ( < 67%) of direct liquid-liquid microextraction. This method has potential in the determination of organic pollutants.
- atrazine /
- in situ ionic liquid formation /
- dispersive liquid-liquid microextraction /
- High Performance Liquid Chromatography

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图 1 水中原位生成离子液体分散微萃取示意图

Figure 1.

下载: 全尺寸图片幻灯片

图 2 离子液体种类(a)、[HMIM]Cl体积(b)对莠去津萃取回收率的影响

Figure 2.

下载: 全尺寸图片幻灯片

图 3 超声时间(a)和离心时间(b)对莠去津萃取回收率的影响

Figure 3.

下载: 全尺寸图片幻灯片

表 1 采用离子液体分散液液微萃取技术提取莠去津的回收率

Table 1. Extraction recovery of atrazine by ILs dispersive liquid-liquid microextraction

萃取剂种类	萃取剂体积 (μL)	分散剂种类	分散剂体积 (μL)	萃取次数	萃取回收率 (%)
[HMIM]PF₆	50	甲醇	200	1	31.3
[OMIM]PF₆	50	甲醇	200	1	38.6
			300	1	39.1
			400	1	35.8
			500	1	33.1
			600	1	27.6
			700	1	25.2
	50	乙腈	300	1	16.8
			400	1	20.9
			500	1	15.5
			600	1	17.1
			700	1	13.9
			60	甲醇	300	1	44.7
	70	400	1		45.9
	80	500	1		51.9
	90	600	1		53.6
	50	甲醇	200	2	47.0
3	50	甲醇	200	66.1

下载: 导出CSV

表 2 实际水样中莠去津加标回收率测定

Table 2. Determination of atrazine in different water

实际样品	加标浓度 (mg/L)	检出浓度 (mg/L)	加标回收率 (%)	标准偏差 (%)
自来水	0.0500	0.0502	100.4	6.9
矿泉水	0.0500	0.0525	105.0	5.6
地下水	0.0500	0.0534	106.7	7.6

下载: 导出CSV

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