Citation: HUANG Huiqiu, HUANG Xun, YU Jingsun. Simultaneous determination of five hypertoxic rodenticides in serum by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(3): 323-328. doi: 10.3724/SP.J.1123.2014.11024 shu

Simultaneous determination of five hypertoxic rodenticides in serum by gas chromatography-mass spectrometry

1.
Pingyang County Center For Disease Prevention and Control, Wenzhou 325400, China

Corresponding author: HUANG Huiqiu,
Received Date: 17 November 2014
Available Online: 30 December 2014

A fast analytical method based on gas chromatography-mass spectrometry (GC-MS) was established for the simultaneous determination of tetramine, fluoroacetamide, sodium fluoroacetate, gliftor Ⅰ and gliftor Ⅱ in serum. At pH 2.0, sodium fluoroacetate was derivatizated at room temperature for 5 min by using N,N-diethyl-p-phenylenediamine as the derivatization reagent and N,N'-dicyclohexylcarbodiimide as the catalyst. The derivative and other rodenticides were extracted with ethyl acetate and concentrated with nitrogen at 50 ℃, then determined by GC-MS in selected ion monitoring (SIM) mode, and quantified with matrix-match standard solutions. The analysis was carried out on an ionic liquid chromatographic capillary column (SLB-IL59, 30 m×0.25 mm×0.20 μm, maximum temperature 300 ℃) at a flow rate of 1.0 mL/min, and the five rodenticides were successfully separated in 15 min when temperature programming was used. The results showed that the calibration curves were linear in the range of 0.01-1.0 mg/L, except for fluoroacetamide (0.02-2.0 mg/L) and tetramine (0.02-10 mg/L), with correlation coefficients (R²) greater than 0.995, and the limits of detection (LODs) were 0.001-0.002 mg/L (S/N=3). The recoveries were 84.0%-110.0% at three different spiked levels, and the relative standard deviations (RSDs) were 2.9%-7.5%(n=6). The method is simple, accurate, highly sensitive and suitable for the detection of the five hypertoxic rodenticides in serum for toxicological purposes.
- gas chromatography-mass spectrometry (GC-MS),
- hypertoxic rodenticide,
- serum
1. [1]
  [1] Liu J Q, Li X M. Chinese Journal of Vector Biology and Control (刘吉起, 李新民. 中国媒介生物学及控制杂志), 2004, 15(2): 148
2. [2]
  [2] Huang H Q. Chinese Journal of Health Laboratory Technology (黄会秋. 中国卫生检验杂志), 2013, 23(15): 3040
3. [3]
  [3] Chen J M, Wang S Y, Qin Y X. Chinese Journal of Health Laboratory Technology (陈京闽, 王生英, 秦迎旭. 中国卫生检验杂志), 2014, 24(18): 2626
4. [4]
  [4] Li Y X, Lin D, Wang X Q, et al. Physical Testing and Chemical Analysis Part B: Chemical Analysis (李艳霞, 林丹, 王贤亲, 等. 理化检验: 化学分册), 2008, 44(7): 640
5. [5]
  [5] Guan F Y, Liu L, Luo Y. Environmental Chemistry (关福玉, 刘力, 罗毅. 环境化学), 1995, 14(3): 196
6. [6]
  [6] Li Y, Yang Z Y, Ma Z P, et al. Forensic Science and Technology (利越, 杨召雨, 马治平, 等. 刑事技术), 2009(6): 27
7. [7]
  [7] Hu P Q, Huang H C, Xiong M. Journal of Environment and Health (胡培勤, 黄辉春, 熊敏. 环境与健康杂志), 2011, 28(6): 542
8. [8]
  [8] Chen B, Liu H L, Rong W G, et al. Chinese Journal of Food Hygiene (陈蓓, 刘华良, 荣维广, 等. 中国食品卫生杂志), 2012, 24(6): 539
9. [9]
  [9] Rong W G, Liu H L, Chen B, et al. Chinese Journal of Analysis Laboratory (荣维广, 刘华良, 陈蓓, 等. 分析试验室), 2013, 32(1): 73
10. [10]
  [10] Zhang J, Lu L B, Yang Y, et al. Journal of Food Safety and Quality (张晶, 卢丽彬, 杨奕, 等. 食品安全质量检测学报), 2013, 4(3): 660
11. [11]
  [11] Ping X H, Gao Y, Yi P. Chinese Journal of Health Laboratory Technology (平小红, 高岩, 伊萍. 中国卫生检验杂志), 2014, 24(11): 1565
12. [12]
  [12] Yuan R, Zou Y J. Capital Journal of Public Health (袁蕊, 邹艳杰. 首都公共卫生), 2014, 8(5): 224
13. [13]
  [13] Guan F Y, Miao Z C, Liu Y T, et al. Military Medical Sciences (关福玉, 缪振春, 刘荫棠, 等. 军事医学科学院院刊), 1997, 21(2): 116
14. [14]
  [14] Liu X P. Chinese Journal of Pharmaceutical Analysis (刘宪平. 药物分析杂志), 2006, 26(7): 978
15. [15]
  [15] Song M, Jia W, Qian D P. Chinese Journal of Health Laboratory Technology (宋鸣, 贾薇, 钱大鹏. 中国卫生检验杂志), 2005, 15(12): 1476
16. [16]
  [16] Lou B B, Xu L M, Hong P. Chinese Journal of Health Laboratory Technology (楼冰冰, 徐陆妹, 洪萍. 中国卫生检验杂志), 2008, 18(9): 1770
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]
  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
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]
  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
5. [5]
  Runjie Li , Hang Liu , Xisheng Wang , Wanqun Zhang , Wanqun Hu , Kaiping Yang , Qiang Zhou , Si Liu , Pingping Zhu , Wei Shao . 氨基酸的衍生及手性气相色谱分离创新实验. University Chemistry, 2025, 40(6): 286-295. doi: 10.12461/PKU.DXHX202407059
6. [6]
  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
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): 100013-0. doi: 10.3866/PKU.WHXB202309036
8. [8]
  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
9. [9]
  Yuanchun Pan , Xinyun Lin , Leyi Yang , Wenya Hu , Dekui Song , Nan Liu . Artificial Intelligence Science Practice: Preparation of Electronic Skin by Chemical Vapor Deposition of Graphene. University Chemistry, 2025, 40(11): 272-280. doi: 10.12461/PKU.DXHX202412052
10. [10]
  Xichen YAO , Shuxian WANG , Yun WANG , Cheng WANG , Chuang ZHANG . Oxygen reduction performance of self?supported Fe/N/C three-dimensional aerogel catalyst layers. Chinese Journal of Inorganic Chemistry, 2025, 41(7): 1387-1396. doi: 10.11862/CJIC.20240384
11. [11]
  Hailang JIA , Yujie LU , Pengcheng JI . Preparation and properties of nitrogen and phosphorus co-doped graphene carbon aerogel supported ruthenium electrocatalyst for hydrogen evolution reaction. Chinese Journal of Inorganic Chemistry, 2025, 41(11): 2327-2336. doi: 10.11862/CJIC.20250021
12. [12]
  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
13. [13]
  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
14. [14]
  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
15. [15]
  Hao Wu , Zhen Liu , Dachang Bai . ¹H NMR Spectrum of Amide Compounds. University Chemistry, 2024, 39(3): 231-238. doi: 10.3866/PKU.DXHX202309020
16. [16]
  Qiuting Zhang , Fan Wu , Jin Liu , Zian Lin . Chromatographic Stationary Phase and Chiral Separation Using Frame Materials. University Chemistry, 2025, 40(4): 291-298. doi: 10.12461/PKU.DXHX202405174
17. [17]
  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
18. [18]
  Fangxuan Liu , Ziyan Liu , Guowei Zhou , Tingting Gao , Wenyu Liu , Bin Sun . 中空结构光催化剂. Acta Physico-Chimica Sinica, 2025, 41(7): 100071-0. doi: 10.1016/j.actphy.2025.100071
19. [19]
  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
20. [20]
  Yue-Zhou Zhu , Kun Wang , Shi-Sheng Zheng , Hong-Jia Wang , Jin-Chao Dong , Jian-Feng Li . Application and Development of Electrochemical Spectroscopy Methods. Acta Physico-Chimica Sinica, 2024, 40(3): 2304040-0. doi: 10.3866/PKU.WHXB202304040

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(359)
HTML views(12)

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