Citation: DING Liping, GUO Jing, ZHENG Ling, CHEN Chuntian, CHEN Zhitao. Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(8): 747-752. doi: 10.3724/SP.J.1123.2013.01033 shu

Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

1.
Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China

Corresponding author: DING Liping,
Received Date: 17 January 2013
Available Online: 21 February 2013
Fund Project: 福建出入境检验检疫局项目(FK2011-61). (FK2011-61)

A method was developed for the determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification (MASP)-gas chromatography (GC)-mass spectrometry (MS). After extracted with 1% acetic acid-acetonitrile, the samples were pretreated with MASP method including extraction, salting-out and purification procedures, and analyzed with GC-MS under the selected ion monitoring (SIM) mode, and then quantified by matrix-match standard solution with external standard method. The results showed good linearity in the range of 2-100 μg/L with the correlation coefficients (r²)not less than 0.999. The average fortified recovery of butene-fipronil in samples was found in the range of 92.2%-97.5% at three fortified levels from 2 to 10 μg/kg, with the relative standard deviations of 2.69%-5.21% (n=6). The limit of detection (S/N=3) for butane-fipronil was 2 μg/kg and the limit of quantification (S/N=10) was 6 μg/kg. The method is simple, rapid and accurate, and could be used for the routine analysis of butane-fipronil in dry samples. Meanwhile, the pyrolysis mechanism of butane-fipronil, as a new substance, is discussed.
- multiple adsorption synchronous purification (MASP),
- gas chromatography-mass spectrometry (GC-MS),
- butene-fipronil,
- residue,
- dry samples
1. [1]
  [1] Dalian RUIZE Pesticide Co., Ltd. World Pesticides (大连瑞泽农药股份有限公司. 世界农药), 2005, 27(5): 49
2. [2]
  [2] Niu H T, Luo W C, Jiang G Q, et al. Acta Phytophylacica Sinica (牛洪涛, 罗万春, 江改青, 等. 植物保护学报), 2007, 34(3): 316
3. [3]
  [3] Li Q, Du J X, Zhang L. China Plant Protection (李前, 杜建雄, 张龙. 中国植保导刊), 2007(11): 39
4. [4]
  [4] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2010, 16(3): 191
5. [5]
  [5] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2011, 17(3): 149
6. [6]
  [6] Feng D Q, Ouyang G P, Kong L H. Guangzhou Chemical Industry (冯道全, 欧阳贵平, 孔令华. 广州化工), 2009, 37(3): 8
7. [7]
  [7] Ding H Y, Xie W, Liu H S. Journal of Instrumental Analysis (丁慧瑛, 谢文, 刘海山. 分析测试学报), 2005, 24(5): 113
8. [8]
  [8] Cao H Q, Shi Y H, Hua R M, et al. Food Science (操海群, 施艳红, 花日茂, 等. 食品科学), 2005, 26(9): 377
9. [9]
  [9] Guo M, Zong L G, Shan Z J, et al. Journal of Agro-Environment Science (郭敏, 宗良纲, 单正军, 等. 农业环境科学学报), 2008, 27(5): 2114
10. [10]
  [10] Wu Z P, Gao W, Yan C R, et al. Modern Agrochemicals (武中平, 高巍, 颜春荣, 等. 现代农药), 2006, 5(2): 21
11. [11]
  [11] Zhou Y, Xu D M, Chen D J, et al. Chinese Journal of Chromatography (周昱, 徐敦明, 陈达捷, 等. 色谱), 2011, 29(7): 656
12. [12]
  [12] Liu Y, Ji M S, Hu R, et al. Journal of Anhui Agriculture Science (刘郁, 纪明山, 胡睿, 等. 安徽农业科学), 2007, 35(18): 5344
13. [13]
  [13] Liu Y, Yu Y H, Bian Y Q, et al. World Pesticides (刘郁, 于亚辉, 边应权, 等. 世界农药), 2008, 30(5): 35
14. [14]
  [14] Cao W Q, Zhao H T, She Y X, et al. Journal of Instrumental Analysis (曹维强, 赵海田, 佘永新, 等. 分析测试学报), 2009, 28(9): 1096
15. [15]
  [15] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
16. [16]
  [16] Gong X M, Dong J, Sun J, et al. Journal of Instrumental Analysis (宫小明, 董静, 孙军, 等. 分析测试学报), 2010, 29(9): 933
17. [17]
  [17] Li C Y, Kong X H, He Q, et al. Food and Nutrition in China (李春艳, 孔祥虹, 何强, 等. 中国食物与营养), 2010(2): 57
18. [18]
  [18] Rawn D F K, Judge J, Roscoe V. Anal Bioanal Chem, 2010, 397: 2525
19. [19]
  [19] Forsberg N D, Wilson G R, Anderson K A. J Agric Food Chem, 2011, 59(15): 8108
20. [20]
  [20] Li X S, Jiang Y P, Shan W L, et al. Bull Environ Contam Toxicol, 2010, 84: 596
21. [21]
  [21] Lucini L, Molinari G P. J Chromatogr Sci, 2011, 49: 709
22. [22]
  [22] Ding L P, Wei Y H. Agrochemicals (丁立平, 魏云昊. 农药), 2011, 50(5): 352
23. [23]
  [23] Xu P J, Gao X S, Tao B, et al. Chinese Journal of Analytical Chemistry (许鹏军, 高晓莎, 陶晡, 等. 分析化学), 2008, 36(11): 1515
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]
  Xiaowu Zhang , Pai Liu , Qishen Huang , Shufeng Pang , Zhiming Gao , Yunhong Zhang . Acid-Base Dissociation Equilibrium in Multiphase System: Effect of Gas. University Chemistry, 2024, 39(4): 387-394. doi: 10.3866/PKU.DXHX202310021
3. [3]
  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
4. [4]
  Jiao CHEN , Yi LI , Yi XIE , Dandan DIAO , Qiang XIAO . Vapor-phase transport of MFI nanosheets for the fabrication of ultrathin b-axis oriented zeolite membranes. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 507-514. doi: 10.11862/CJIC.20230403
5. [5]
  Fang Niu , Rong Li , Qiaolan Zhang . Analysis of Gas-Solid Adsorption Behavior in Resistive Gas Sensing Process. University Chemistry, 2024, 39(8): 142-148. doi: 10.3866/PKU.DXHX202311102
6. [6]
  Qianqian Zhong , Yucui Hao , Guotao Yu , Lijuan Zhao , Jingfu Wang , Jian Liu , Xiaohua Ren . Comprehensive Experimental Design for the Preparation of the Magnetic Adsorbent Based on Enteromorpha Prolifera and Its Utilization in the Purification of Heavy Metal Ions Wastewater. University Chemistry, 2024, 39(8): 184-190. doi: 10.3866/PKU.DXHX202312013
7. [7]
  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-. doi: 10.3866/PKU.WHXB202309036
8. [8]
  Xuanzhu Huo , Yixi Liu , Qiyu Wu , Zhiqiang Dong , Chanzi Ruan , Yanping Ren . Integrated Experiment of “Electrolytic Preparation of Cu₂O and Gasometric Determination of Avogadro’s Constant: Implementation, Results, and Discussion: A Micro-Experiment Recommended for Freshmen in Higher Education at Various Levels Across the Nation. University Chemistry, 2024, 39(3): 302-307. doi: 10.3866/PKU.DXHX202308095
9. [9]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . 液相法制备硫化物固体电解质及其在全固态锂电池中的应用. Acta Physico-Chimica Sinica, 2025, 41(1): 2309019-. doi: 10.3866/PKU.WHXB202309019
10. [10]
  Zian Lin , Yingxue Jin . Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry (MALDI-MS) for Disease Marker Screening and Identification: A Comprehensive Experiment Teaching Reform in Instrumental Analysis. University Chemistry, 2024, 39(11): 327-334. doi: 10.12461/PKU.DXHX202403066
11. [11]
  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
12. [12]
  Zehua Zhang , Haitao Yu , Yanyu Qi . 多重共振TADF分子的设计策略. Acta Physico-Chimica Sinica, 2025, 41(1): 2309042-. doi: 10.3866/PKU.WHXB202309042
13. [13]
  Wenkai Chen , Yunjia Shen , Xiangmeng Kong , Yanli Zeng . Quantum Chemistry Calculation of Key Physical Quantity in Circularly Polarized Luminescence: Introducing an Exploratory Computational Chemistry Experiment. University Chemistry, 2025, 40(3): 83-91. doi: 10.12461/PKU.DXHX202405018
14. [14]
  Wei Li , Guoqiang Feng , Ze Chang . Teaching Reform of X-ray Diffraction Using Synchrotron Radiation in Materials Chemistry. University Chemistry, 2024, 39(3): 29-35. doi: 10.3866/PKU.DXHX202308060
15. [15]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
16. [16]
  Hao Wu , Zhen Liu , Dachang Bai . ¹H NMR Spectrum of Amide Compounds. University Chemistry, 2024, 39(3): 231-238. doi: 10.3866/PKU.DXHX202309020
17. [17]
  Xiaoning TANG , Shu XIA , Jie LEI , Xingfu YANG , Qiuyang LUO , Junnan LIU , An XUE . Fluorine-doped MnO₂ with oxygen vacancy for stabilizing Zn-ion batteries. Chinese Journal of Inorganic Chemistry, 2024, 40(9): 1671-1678. doi: 10.11862/CJIC.20240149
18. [18]
  Shahua Huang , Xiaoming Guo , Lin Lin , Guangping Chang , Sheng Han , Zuxin Zhou . Application of “Integration of Industry and Education” in Engineering Chemistry: Improvement of the Pesticide Fipronil Production. University Chemistry, 2024, 39(3): 199-204. doi: 10.3866/PKU.DXHX202309064
19. [19]
  Xiaofeng Xia , Jielian Zhu . Innovative Comprehensive Experimental Design: Synthesis of 6-Fluoro-N-benzoyl Tetrahydroquinoline. University Chemistry, 2024, 39(10): 344-352. doi: 10.12461/PKU.DXHX202405063
20. [20]
  Tingting Yu , Si Chen , Lianglong Sun , Tongtong Shi , Kai Sun , Xin Wang . Comprehensive Experimental Design for the Photochemical Synthesis, Analysis, and Characterization of Difluoropyrroles. University Chemistry, 2024, 39(11): 196-203. doi: 10.3866/PKU.DXHX202401022

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(166)
HTML views(10)

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