Citation: LI Liping, FAN Sai, ZHAO Rong, LI Bing, LIU Wei, WU Guohua. Determination of zearalanol and related mycotoxins in pork by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(7): 703-708. doi: 10.3724/SP.J.1123.2012.12033 shu

Determination of zearalanol and related mycotoxins in pork by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

1.
Institute of Nutrition and Food Hygiene, Beijing Center for Disease Control & Prevention, Beijing 100013, China

Corresponding author: ZHAO Rong,
Received Date: 18 December 2012

Fund Project: 北京市自然科学基金项目(7102087). (7102087)

A method was established for the determination of six compounds of zearalanol and related mycotoxins in pork and its products. After hydrolysis of the target compounds in the pork by β-glucosidase/sulfatase, they were extracted with methanol aqueous solution and further purified by an HLB column. The separation was performed on a BEH C18 column with gradient elution using acetonitrile-water as mobile phases. The analytes were determined by mass spectrometry using electrospray ionization (ESI) in negative scan mode and multiple reaction monitoring (MRM) mode. α-Zearalenol-D7 and β-zearalenol-D7 were used as internal standards. The good linearities (r >0.999) were achieved for the six compounds over the range of 1.0-100 μ g/L based on the internal standard calibration. The detection limits of the method were 0.03-0.09 μ g/kg. The mean recoveries of the six target compounds spiked at three levels from 1.0-10.0 μ g/kg ranged from 76.7% to 100.5% with the relative standard deviations (RSDs) less than 20%. The proposed method is simple, sensitive, reproducible, and complies with the regulations for the determination of trace contaminant residues in food matrices.
- solid-phase extraction (SPE),
- ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- zearalanol,
- mycotoxin
1. [1]
  [1] Kennedy D G, Hewitt S A, McEvoy J D G, et al. Food Addit Contam, 1998, 15(4): 393
2. [2]
  [2] Wang S, Wang X H. Food Addit Contam, 2007, 24(6): 573
3. [3]
  [3] Kleinova M, Zollner P, Kahlbacher H, et al. J Agric Food Chem, 2002, 50(17): 4769
4. [4]
  [4] Richardson K E, Hagler W M J, Mirocha C J. J Agric Food Chem, 1985, 33(5): 862
5. [5]
  [5] Dong M, He X J, Tulayakul P, et al. Toxicon, 2010, 55(2/3): 523
6. [6]
  [6] Tsakmakidis I A, Lymberopoulos A G, Khalifa T A A, et al. J Appl Toxicol, 2008, 28(5): 681
7. [7]
  [7] Draughon F A, Churchville D C. Phytopathology, 1985, 75(5): 553
8. [8]
  [8] Joint FAO/WHO Expert Committee on Food Additives (JECFA). WHO Food Additives Series. Geneva: World Health Organization, 2000: 44
9. [9]
  [9] Bulletin No.235, Ministry of Agriculture, PR China. Maximum Residue Limits of Veterinary Drugs in Food of Animal Origin (中华人民共和国农业部第235号公告: 动物源性食品中兽药最高残留限量). 2002: Appendix 4
10. [10]
  [10] The Council of the European Union. Council Directive 96/22/EC of 29 April 1996 Concerning the Prohibition on the Use in Stock-farming of Certain Substances Having Hormonal or Thyrostaic Action and of Beta-agonists and Repealing Directives 81/602/EEC, 88/146/EEC and 88/299/EC. Off J Eur Comm, L125: 3
11. [11]
  [11] Food and Agriculture Organization of the United Nations (FAO). Worldwide Regulations for Mycotoxins in Food and Feed in 2003. Rome, 2004. [2012-12-18]. http://www.fao.org/docrep/007/y5499e/y5499e00.htm
12. [12]
  [12] Sydenham E W, Gelderblom W C A, Thiel P G, et al. J Agric Food Chem, 1990, 38(1): 285
13. [13]
  [13] Burmistrova N A, Goryacheva I Y, Basova E Y, et al. Anal Bioanal Chem, 2009, 395(5): 1301
14. [14]
  [14] Medina M B, Nagdy N. J Chromatogr B, 1993, 614(2): 315
15. [15]
  [15] Zeng H Y, Li Y Q, Jing H Q. Chinese Journal of Analytical Chemistry (曾红燕, 黎源倩, 敬海泉. 分析化学), 2006, 34(3): 351
16. [16]
  [16] Cavaliere C, D'Ascenzo G, Foglia P, et al. Food Chem, 2005, 92(3): 559
17. [17]
  [17] You L N, Li X L, Xi C X, et al. Chinese Journal of Chromatography (游丽娜, 李贤良, 郗存显, 等. 色谱), 2012, 30(10): 1021
18. [18]
  [18] Zhang W, Wang J P, Shen J Z, et al. Acta Veterinaria et Zootechnica Sinica (张伟, 王建平, 沈建忠, 等. 畜牧兽医学报), 2007, 38(5): 513
19. [19]
  [19] Meng J, Zhang J, Zhang N, et al. Chinese Journal of Chromatography (孟娟, 张晶, 张楠, 等. 色谱), 2010, 28(6): 601
20. [20]
  [20] Hartmann N, Erbs M, Wettstein F E, et al. J Chromatogr A, 2007, 1138(1/2): 132
21. [21]
  [21] Xia X, Li X W, Ding S Y, et al. J Chromatogr A, 2009, 1216(12): 2587
22. [22]
  [22] Ren Y, Zhang Y, Shao S, et al. J Chromatogr A, 2007, 1143(1/2): 48
23. [23]
  [23] Bulletin No.1025, Ministry of Agriculture, PR China (中华人民共和国农业部第1025号公告). 2008
24. [24]
  [24] GB/T 21982-2008
25. [25]
  [25] Commission Decision 2002/657/EC of 12 August 2002. Implementing Council Directive 96/23/EC Concerning the Performance of Analytical Methods and the Interpretation of Results (2002). Off J Eur Comm, L221: 8
1. [1]
  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
2. [2]
  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
3. [3]
  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
4. [4]
  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
5. [5]
  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
6. [6]
  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
7. [7]
  Chunai Dai , Yongsheng Han , Luting Yan , Zhen Li , Yingze Cao . Ideological and Political Design of Solid-liquid Contact Angle Measurement Experiment. University Chemistry, 2024, 39(2): 28-33. doi: 10.3866/PKU.DXHX202306065
8. [8]
  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
9. [9]
  Zhiwen HU , Weixia DONG , Qifu BAO , Ping LI . Low-temperature synthesis of tetragonal BaTiO₃ for piezocatalysis. Chinese Journal of Inorganic Chemistry, 2024, 40(5): 857-866. doi: 10.11862/CJIC.20230462
10. [10]
  Haiyang Zhang , Yanzhao Dong , Haojie Li , Ruili Guo , Zhicheng Zhang , Jiangjiexing Wu . Exploring the Integration of Chemical Engineering Principle Experiment with Cutting-Edge Research Achievements. University Chemistry, 2024, 39(10): 308-313. doi: 10.12461/PKU.DXHX202405035
11. [11]
  Yuyang Xu , Ruying Yang , Yanzhe Zhang , Yandong Liu , Keyi Li , Zehui Wei . Research Progress of Aflatoxins Removal by Modern Optical Methods. University Chemistry, 2024, 39(11): 174-181. doi: 10.12461/PKU.DXHX202402064
12. [12]
  Zhuoming Liang , Ming Chen , Zhiwen Zheng , Kai Chen . Multidimensional Studies on Ketone-Enol Tautomerism of 1,3-Diketones By ¹H NMR. University Chemistry, 2024, 39(7): 361-367. doi: 10.3866/PKU.DXHX202311029
13. [13]
  Lihui Jiang , Wanrong Dong , Hua Yang , Yongqing Xia , Hongjian Peng , Jun Yuan , Xiaoqian Hu , Zihan Zeng , Yingping Zou , Yiming Luo . Study on Extraction of p-Hydroxyacetophenone. University Chemistry, 2024, 39(11): 259-268. doi: 10.12461/PKU.DXHX202402056
14. [14]
  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
15. [15]
  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
16. [16]
  Yiling Wu , Peiyao Jin , Shenyue Tian , Ji Zhang . The Star of Sugar Substitutes: An Interview of Erythritol. University Chemistry, 2024, 39(9): 22-27. doi: 10.12461/PKU.DXHX202404034
17. [17]
  Aili Feng , Xin Lu , Peng Liu , Dongju Zhang . Computational Chemistry Study of Acid-Catalyzed Esterification Reactions between Carboxylic Acids and Alcohols. University Chemistry, 2025, 40(3): 92-99. doi: 10.12461/PKU.DXHX202405072
18. [18]
  Zhanggui DUAN , Yi PEI , Shanshan ZHENG , Zhaoyang WANG , Yongguang WANG , Junjie WANG , Yang HU , Chunxin LÜ , Wei ZHONG . Preparation of UiO-66-NH₂ supported copper catalyst and its catalytic activity on alcohol oxidation. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 496-506. doi: 10.11862/CJIC.20230317
19. [19]
  Xinhao Yan , Guoliang Hu , Ruixi Chen , Hongyu Liu , Qizhi Yao , Jiao Li , Lingling Li . Polyethylene Glycol-Ammonium Sulfate-Nitroso R Salt System for the Separation of Cobalt (II). University Chemistry, 2024, 39(6): 287-294. doi: 10.3866/PKU.DXHX202310073
20. [20]
  Yifeng TAN , Ping CAO , Kai MA , Jingtong LI , Yuheng WANG . Synthesis of pentaerythritol tetra(2-ethylthylhexoate) catalyzed by h-MoO₃/SiO₂. Chinese Journal of Inorganic Chemistry, 2024, 40(11): 2155-2162. doi: 10.11862/CJIC.20240147

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(197)
HTML views(5)

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