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

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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
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