Citation: CAI Zhibin, SUN Jinying, XU Xiaoyan, ZHANG Ying, LAI Jianhui, LIU Jinming. QuEChERS Purification with HPLC-MS/MS for Rapid Confirmation in Acute Clenbuterol Poisoning Case Sample[J]. Chinese Journal of Applied Chemistry, ;2019, 36(7): 832-838. doi: 10.11944/j.issn.1000-0518.2019.07.180391 shu

QuEChERS Purification with HPLC-MS/MS for Rapid Confirmation in Acute Clenbuterol Poisoning Case Sample

Longgang District Center for Disease Control and Prevention, Shenzhen, Guangdong 518172, China

Corresponding author: CAI Zhibin, 1005754603@qq.com
Received Date: 5 December 2018
Revised Date: 30 January 2019
Accepted Date: 8 March 2019

Fund Project: the Scientific Research Project of Shenzhen Health and Family Planning System 201303222Supported by the Scientific Research Project of Shenzhen Health and Family Planning System(No.201303222), Science and Technology Projects of Shenzhen Longgang District(No.LG20140515115239)Science and Technology Projects of Shenzhen Longgang District LG20140515115239

Figures(2)

The pretreatment procedure of enzymatic hydrolysis and extraction coupled with solid phase extraction(SPE) purification is usually employed for the determination of β-agonists by high performance liquid chromatography(HPLC) with tandam mass spetroscopy(MS) in food originated from animals. In this study, a HPLC-MS/MS with QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safe) purification procedures was developed for the determination of terbutaline, salbutamol, ractopamine and clenbuterol in food of animal origin using both acid hydrolysis extraction method and enzymatic hydrolysis extraction method in food poisoning event caused by clenbuterol and analogs. Using enzymatic hydrolysis extraction with QuEChERS purification and electrospray ionization mass spectrometry in positive mode adopting multiple reaction monitoring(MRM) mode, four analytes were analyzed in the range of 1.0~20.0 μg/L with correlation coefficients(R) higher than 0.999. The limit of detection(LOD) and the limit of quantification(LOQ) was 0.1 μg/kg and 0.3 μg/kg, respectively, and recoveries for 4 β₂-agonists in pork and beef samples ranged from 78.5% to 112% with relative standard deviation(RSD) of 2.8%~8.9%. When acid hydrolysis extraction was used alternatively, the pretreatment time was shortened greatly, but the result for ractopamine was slightly lower than that using the enzymatic hydrolysis extraction procedure. The combined use of two pretreatment procedures will promote the emergency response in real food poisoning case caused by clenbuterol and analogs.
1. [1]
  LIU Xianjun, WANG Yihong, LI Bangrui. Determination of 26β Agonists in Liver of Pigs and Ducks Using Ultra Pressure Liquid Chromatography Tandem Quadrupole Mass Spectrometry[J]. Chinese J Food Hygiene, 2015,27(3):265-270.
2. [2]
  YE Ni, SUN Lei, YIN Hui. Determination of β Agonists in Animal Derived Food by UPLC-MS/MS[J]. Chinese J Veterin Drug, 2015,49(9):51-59.
3. [3]
  XIONG Lin, LI Weihong, GAO Yaqin. A Review of Inspection Technology of β Agonist Drug Residues in Meat[J]. J Food Saf Food Qual, 2015,6(2):528-533.
4. [4]
  China's Ministry of Agriculture Bulletin No.1025-18-2008, the Catalogue of Forbidden Drug in Feed and Drinking Water of Animal[Z]. 2002(in Chinese).
5. [5]
  DONG Fengguang, WANG Guiqiang, GONG Chunbo. Pollution Status and Risk Assessment of Heavy Metals and β-Receptor Agonist in Commercially Available Livestock and Poultry Meat in Yantai City from 2012-2017[J]. Occup Health, 2018,34(6):764-768.
6. [6]
  ZHOU Yuerong, LI Danni, GU Xin. Determination of 11β₂-Agonists Residues in Swine and Chicken Manure by Enzyme Linked Immunosorbent Assay[J]. Chinese J Veterin Drug, 2015,49(8):39-45.
7. [7]
  YUE Hanxiao, LEI Wen, DU Xiaoning. Multi-residue Analysis of 4β-Agonists in Pork Using Isotope Dilution Gas Chromatography-Tandem Mass Spectrometry[J]. J Chinese Mass Spectrom Soc, 2018,39(1):61-68.
8. [8]
  WANG Quanshuai, SUN Weiming, LIU Jianrong. Determination of Four Clenbuterol Residues in Pork by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry[J]. Occup Health, 2015,31(2):181-183.
9. [9]
  CAI Yuzhi, LUO Xiaoyan, SU Wenzhou. Clenbuterol Hydrochloride Residue Determination by High Performance Liquid Chromatography in Pork[J]. Chinese J Lab Technol, 2002,12(2):193-194. doi: 10.3969/j.issn.1004-8685.2002.02.036
10. [10]
  Li L B, Du H W, Yu H. Application of Ionic Liquid as Additive in Determination of Three β Agonists by Capillary Electrophoresis with Amperometric Detection[J]. Electrophoresis, 2013,34:277-283. doi: 10.1002/elps.v34.2
11. [11]
  Wang G M, Zhao J, Peng T. Matrix Effects in the Determination of β Receptor Agonists in Animal-Derived Foodstuffs by Ultra-Performance Liquid Chromatography Tadem Mass Spectrometry with Immunoaffinity Solid-Phase Extraction[J]. J Sep Sci, 2013,36:796-802. doi: 10.1002/jssc.v36.4
12. [12]
  Suo D C, Zhao G L, Wang P L. Simultaneous Determination of β Agonists and Psychiatric Drugs in Feeds by LC-MS-MS[J]. J Chromatogr Sci, 2014,52(7):604-608. doi: 10.1093/chromsci/bmt084
13. [13]
  LIU Guihua, MAO Lisha, ZHU Zhou. Determination of Residues of Nine β Agonists in Edible Meat and Liver by Liquid Chromatography Tandem Mass Spectrometry[J]. South China J Prev Med, 2014,40(5):425-430.
14. [14]
  SHI Na, HAO Jie, JIANG Jie. Simultaneous Determination of 35β-agonist and 11β-Blocker Residues in Animal-Origin Foods by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Anal Instrum, 2018,1:20-31.
15. [15]
  QU Bin, GENG Shiwei, LU Guiping. Rapid Determination of β Agonists Residuals in Pig Liver by Liquid Chromatography Tandem Mass Spectrometry Combined with Novel QuEChERS Method[J]. J Food Saf Food Qual, 2015,6(12):4747-4754.
16. [16]
  LI Lei, LI Haichang, GAO Jing. Determination of 8β Agonists by QuEChERS EMR-Lipid-LC/MS/MS[J]. Food Res Dev, 2016,37(9):178-182. doi: 10.3969/j.issn.1005-6521.2016.09.042
17. [17]
  ZHU Weixia, YANG Yizhou, GUO Huiling. Quick Determination of 16β-Agonist Residues in Pig Urine by Turboflow Cation Online Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry[J]. J Instrum Anal, 2015,34(7):802-806. doi: 10.3969/j.issn.1004-4957.2015.07.008
1. [1]
  Yukun Chang , Haoqin Huang , Baolei Wang . Preparation of Trans-Cinnamic Acid via “One-Pot” Protocol of Aldol Condensation-Hydrolysis Reaction: Recommending an Improved Organic Synthesis Experiment. University Chemistry, 2024, 39(4): 322-328. doi: 10.3866/PKU.DXHX202309095
2. [2]
  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
3. [3]
  Yaling Chen . Basic Theory and Competitive Exam Analysis of Dynamic Isotope Effect. University Chemistry, 2024, 39(8): 403-410. doi: 10.3866/PKU.DXHX202311093
4. [4]
  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
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]
  Jiahe LIU , Gan TANG , Kai CHEN , Mingda ZHANG . Effect of low-temperature electrolyte additives on low-temperature performance of lithium cobaltate batteries. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 719-728. doi: 10.11862/CJIC.20250023
7. [7]
  Ran Yu , Chen Hu , Ruili Guo , Ruonan Liu , Lixing Xia , Cenyu Yang , Jianglan Shui . Catalytic Effect of H₃PW₁₂O₄₀ on Hydrogen Storage of MgH₂. Acta Physico-Chimica Sinica, 2025, 41(1): 100001-0. doi: 10.3866/PKU.WHXB202308032
8. [8]
  Yu Peng , Jiawei Chen , Yue Yin , Yongjie Cao , Mochou Liao , Congxiao Wang , Xiaoli Dong , Yongyao Xia . Tailored cathode electrolyte interphase via ethylene carbonate-free electrolytes enabling stable and wide-temperature operation of high-voltage LiCoO₂. Acta Physico-Chimica Sinica, 2025, 41(8): 100087-0. doi: 10.1016/j.actphy.2025.100087
9. [9]
  Liwei Wang , Guangran Ma , Li Wang , Fugang Xu . A Comprehensive Analytical Chemistry Experiment: Colorimetric Detection of Vitamin C Using Nanozyme and Smartphone. University Chemistry, 2024, 39(8): 255-262. doi: 10.3866/PKU.DXHX202312094
10. [10]
  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
11. [11]
  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
12. [12]
  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
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]
  Xiyuan Zhang , Rui Dong , Yang Yang , Jiapeng Ding , Zhiwei Miao . Palladium-Catalyzed Tandem Cyclization of 4-Vinylbenzoxazinone and Indene-2-carbaldehyde: A Comprehensive Organic Chemistry Experiment. University Chemistry, 2025, 40(9): 361-367. doi: 10.12461/PKU.DXHX202410062
15. [15]
  Mengyang LI , Hao XU , Zhonghao NIU , Chunhua GONG , Weihui ZHONG , Jingli XIE . Highly effective catalytic synthesis of β-amino alcohols by using viologen-polyoxometalate hybrid materials. Chinese Journal of Inorganic Chemistry, 2025, 41(7): 1294-1300. doi: 10.11862/CJIC.20250080
16. [16]
  Jingzhao Cheng , Shiyu Gao , Bei Cheng , Kai Yang , Wang Wang , Shaowen Cao . Construction of 4-Amino-1H-imidazole-5-carbonitrile Modified Carbon Nitride-Based Donor-Acceptor Photocatalyst for Efficient Photocatalytic Hydrogen Evolution. Acta Physico-Chimica Sinica, 2024, 40(11): 2406026-0. doi: 10.3866/PKU.WHXB202406026
17. [17]
  Quanliang Chen , Zhaohui Zhou . Research on the Active Site of Nitrogenase over Fifty Years. University Chemistry, 2024, 39(7): 287-293. doi: 10.3866/PKU.DXHX202310133
18. [18]
  Peng XU , Shasha WANG , Nannan CHEN , Ao WANG , Dongmei YU . Preparation of three-layer magnetic composite Fe₃O₄@polyacrylic acid@ZiF-8 for efficient removal of malachite green in water. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 544-554. doi: 10.11862/CJIC.20230239
19. [19]
  Heng Zhang . Determination of All Rate Constants in the Enzyme Catalyzed Reactions Based on Michaelis-Menten Mechanism. University Chemistry, 2024, 39(4): 395-400. doi: 10.3866/PKU.DXHX202310047
20. [20]
  Qing Li , Guangxun Zhang , Yuxia Xu , Yangyang Sun , Huan Pang . P-Regulated Hierarchical Structure Ni₂P Assemblies toward Efficient Electrochemical Urea Oxidation. Acta Physico-Chimica Sinica, 2024, 40(9): 2308045-0. doi: 10.3866/PKU.WHXB202308045

Get Citation

PDF

XML

Metrics

PDF Downloads(3)
Abstract views(598)
HTML views(103)

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