Citation: WANG Yu, ZHU Chenghua, ZOU Xiaoli, HUANG Lizhi, YAN Dong. Solvent demulsification-dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with gas chromatography-mass spectrometry for simultaneous determination of organochlorine pesticides in aqueous samples[J]. Chinese Journal of Chromatography, ;2013, 31(11): 1076-1080. doi: 10.3724/SP.J.1123.2013.06008 shu

Solvent demulsification-dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with gas chromatography-mass spectrometry for simultaneous determination of organochlorine pesticides in aqueous samples

1.
West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China

Corresponding author: ZOU Xiaoli,
Received Date: 4 June 2013
Available Online: 11 July 2013
Fund Project: 四川大学本科科研训练项目(20131462,504). (20131462,504)

A novel method for simultaneous determination of eight organochlorine pesticides in aqueous samples by solvent demulsification-dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with gas chromatography-mass spectrometry (GC-MS) was established. A mixture of extractant (n-hexadecane) and dispersive agent (acetone) at the ratio of 1/5 (v/v) was injected into aqueous sample to form an emulsion and an extraction process was accomplished. The demulsifier (750 μ L acetone) was then injected to break up the emulsion. The two phases were separated quickly without centrifugation. After being solidified in an ice-bath, the upper layer (n-hexadecane) was transferred into an Eppendorf tube and analyzed by GC-MS after melted at room temperature. Factors affecting extraction efficiency such as the type and volume of extractant, dispersive agent and demulsifier, also ionic strength and pH value of extraction system were studied. Under the optimized conditions, the working curve of the proposed method provided a good linearity in the range of 0.025-2.00 μg/L (r=0.9995-0.9999). The detection limits of the organochlorine pesticides calculated by Hubaux-Vos method were 0.012-0.024 μg/L and the relative standard deviations (RSDs) ranged from 3.15% to 4.53%. The enrichment factors (EF) were 96-101. When the method was applied to the determination of farmland water, the average spiked recoveries were 96.77%-102.93% with the relative standard deviations of 2.68%-4.86%. The proposed method is sensitive and fast. It also has the advantage of little organic solvent consumption so that it is friendly to environment and suitable for batch analysis of organochlorine pesticides in aqueous samples. Meanwhile, it provides technical and methodological support for achieving the automation of sample pretreatment.
1. [1]
  [1] Liu H H, Dasgupta P K. Trends Anal Chem, 1996, 68(11): 1817
2. [2]
  [2] Pedersen-Bjergaard S, Rasumussen K E. Anal Chem, 1999, 71(14): 2650
3. [3]
  [3] Rezaee M, Assadi Y, Hosseini M R M, et al. J Chromatogr A, 2006, 1116: 1
4. [4]
  [4] Zanjani M R K, Yamini Y, Shariati S, et al. Anal Chim Acta, 2007, 585(2): 286
5. [5]
  [5] Leong M I, Huang S D. J Chromatogr A, 2008, 1211: 8
6. [6]
  [6] Saleh A, Yamini Y, Faraji M, et al. J Chromatogr A, 2009, 1216(39): 6673
7. [7]
  [7] Zacharis C K, Tzanavaras P D, Roubos K, et al. J Chromatogr A, 2010, 1217: 5896
8. [8]
  [8] Chen H, Chen R W, Li S Q. J Chromatogr A, 2010, 1217: 1244
9. [9]
  [9] Guo L, Lee H K. J Chromatogr A, 2011, 1218: 5040
10. [10]
  [10] Zhu B Q, Chen H, Li S Q. Chinese Journal of Chromatography (祝本琼, 陈浩, 李胜清. 色谱), 2012, 30(2): 201
11. [11]
  [11] Hubaux A, Vos G. Anal Chem, 1970, 42(8): 849
12. [12]
  [12] Leong M I, Huang S D. J Chromatogr A, 2009, 1216: 7645
1. [1]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
2. [2]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
3. [3]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
4. [4]
  Zongyuan Chen , ChunSheng Shi , Yiwen Li , Ganlin Zu , Qiang Jin , Haishan Wang , Fujun Wang , Dekun Yan , Zhijun Guo , Wangsuo Wu . Measurement of Uranium Isotopes in Environmental Water Samples by Alpha-Spectroscopy: Design of an Undergraduate Radiochemistry Experiment. University Chemistry, 2025, 40(4): 353-358. doi: 10.12461/PKU.DXHX202406103
5. [5]
  Chongjing Liu , Yujian Xia , Pengjun Zhang , Shiqiang Wei , Dengfeng Cao , Beibei Sheng , Yongheng Chu , Shuangming Chen , Li Song , Xiaosong Liu . Understanding Solid-Gas and Solid-Liquid Interfaces through Near Ambient Pressure X-Ray Photoelectron Spectroscopy. Acta Physico-Chimica Sinica, 2025, 41(2): 100013-0. doi: 10.3866/PKU.WHXB202309036
6. [6]
  Yifan Xie , Liyun Yao , Ruolin Yang , Yuxing Cai , Yujie Jin , Ning Li . Exploration and Practice of Online and Offline Hybrid Teaching Mode in High-Performance Liquid Chromatography Experiment. University Chemistry, 2025, 40(11): 100-107. doi: 10.12461/PKU.DXHX202412133
7. [7]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries. Acta Physico-Chimica Sinica, 2025, 41(1): 100004-0. doi: 10.3866/PKU.WHXB202309019
8. [8]
  Qiuyang LUO , Xiaoning TANG , Shu XIA , Junnan LIU , Xingfu YANG , Jie LEI . Application of a densely hydrophobic copper metal layer in-situ prepared with organic solvents for protecting zinc anodes. Chinese Journal of Inorganic Chemistry, 2024, 40(7): 1243-1253. doi: 10.11862/CJIC.20240110
9. [9]
  Zhenhuan Wang , Weifei Wei , Ruijie Ma , Dou Luo , Zhanxiang Chen , Jun Zhang , Liyang Yu , Gang Li , Zhenghui Luo . Core cyanation of benzo[a]phenazine acceptor enables 19.04% binary organic solar cells with green solvent compatibility. Acta Physico-Chimica Sinica, 2026, 42(2): 100182-0. doi: 10.1016/j.actphy.2025.100182
10. [10]
  Qilong Fang , Yiqi Li , Jiangyihui Sheng , Quan Yuan , Jie Tan . Magical Pesticide Residue Detection Test Strips: Aptamer-based Lateral Flow Test Strips for Organophosphorus Pesticide Detection. University Chemistry, 2024, 39(5): 80-89. doi: 10.3866/PKU.DXHX202310004
11. [11]
  Fan Wu , Wenchang Tian , Jin Liu , Qiuting Zhang , YanHui Zhong , Zian Lin . Core-Shell Structured Covalent Organic Framework-Coated Silica Microspheres as Mixed-Mode Stationary Phase for High Performance Liquid Chromatography. University Chemistry, 2024, 39(11): 319-326. doi: 10.12461/PKU.DXHX202403031
12. [12]
  Hao Chen , Dongyue Yang , Gang Huang , Xinbo Zhang . Progress on Liquid Organic Electrolytes of Li-O₂ Batteries. Acta Physico-Chimica Sinica, 2024, 40(7): 2305059-0. doi: 10.3866/PKU.WHXB202305059
13. [13]
  Jiandong Liu , Xin Li , Daxiong Wu , Huaping Wang , Junda Huang , Jianmin Ma . Anion-Acceptor Electrolyte Additive Strategy for Optimizing Electrolyte Solvation Characteristics and Electrode Electrolyte Interphases for Li||NCM811 Battery. Acta Physico-Chimica Sinica, 2024, 40(6): 2306039-0. doi: 10.3866/PKU.WHXB202306039
14. [14]
  Ruonan Li , Shijie Liang , Yunhua Xu , Cuifen Zhang , Zheng Tang , Baiqiao Liu , Weiwei Li . Chlorine-Substituted Double-Cable Conjugated Polymers with Near-Infrared Absorption for Low Energy Loss Single-Component Organic Solar Cells. Acta Physico-Chimica Sinica, 2024, 40(8): 2307037-0. doi: 10.3866/PKU.WHXB202307037
15. [15]
  Ke Qiu , Fengmei Wang , Mochou Liao , Kerun Zhu , Jiawei Chen , Wei Zhang , Yongyao Xia , Xiaoli Dong , Fei Wang . A Fumed SiO₂-based Composite Hydrogel Polymer Electrolyte for Near-Neutral Zinc-Air Batteries. Acta Physico-Chimica Sinica, 2024, 40(3): 2304036-0. doi: 10.3866/PKU.WHXB202304036
16. [16]
  Mengzhen JIANG , Qian WANG , Junfeng BAI . Research progress on low-cost ligand-based metal-organic frameworks for carbon dioxide capture from industrial flue gas. Chinese Journal of Inorganic Chemistry, 2025, 41(1): 1-13. doi: 10.11862/CJIC.20240355
17. [17]
  Chengshan Yuan , Xiaolong Li , Xiuping Yang , Xiangfeng Shao , Zitong Liu , Xiaolei Wang , Yongwen Shen . Standardized Operational Guidelines for Mixed-Solvent Recrystallization in Organic Chemistry Experiment. University Chemistry, 2025, 40(5): 122-127. doi: 10.12461/PKU.DXHX202504073
18. [18]
  Houjin Li , Lin Wu , Xingwen Sun , Yuan Zheng , Zhanxiang Liu , Shuanglian Cai , Ying Xiong , Guangao Yu , Qingwen Liu , Jie Han , Xin Du , Chengshan Yuan , Qihan Zhang , Jianrong Zhang , Shuyong Zhang . Basic Operations and Specification Suggestions for Organic Chemical Chromatography Experiments. University Chemistry, 2025, 40(5): 93-105. doi: 10.12461/PKU.DXHX202408100
19. [19]
  Zhanxiang Liu , Chengshan Yuan , Jie Han , Shuanglian Cai , Qihan Zhang , Lin Wu , Yuan Zheng , Xingwen Sun , Qingwen Liu , Ying Xiong , Guangao Yu , Xin Du , Houjin Li , Jianrong Zhang , Shuyong Zhang . Recommendations for Basic Operations and Standards for Organic Chemical Extraction and Washing Experiments. University Chemistry, 2025, 40(5): 55-65. doi: 10.12461/PKU.DXHX202410039
20. [20]
  Qianlang Wang , Jijun Sun , Qian Chen , Quanqin Zhao , Baojuan Xi . The Appeal of Organophosphorus Compounds: Clearing Their Name. University Chemistry, 2025, 40(4): 299-306. doi: 10.12461/PKU.DXHX202405205

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(625)
HTML views(8)

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