Citation: LUO Huitai, HUANG Xiaolan, WU Huiqin, ZHU Zhixin, HUANG Fang, LIN Xiaoshan, ZHANG Qiuyan, MA Yefen. Simultaneous determination of 26 β-agonists in pork by dispersive solid-phase extraction and isotope dilution-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(5): 481-489. doi: 10.3724/SP.J.1123.2016.01015 shu

Simultaneous determination of 26 β-agonists in pork by dispersive solid-phase extraction and isotope dilution-high performance liquid chromatography-tandem mass spectrometry

1.
China National Analytical Center(Guangzhou), Guangdong Provincial Public Laboratory of Analysis and Testing Technology, Guangzhou 510070, China

Corresponding author: HUANG Xiaolan,
Received Date: 12 January 2016

Fund Project: 广东省科技计划项目(2014B070705001) (2014B070705001)广州市科技计划项目(11BppZXcc6100034). (11BppZXcc6100034)

A method has been developed and validated for the determination of 26 β-agonists in pork using dispersive solid-phase extraction (dSPE) coupled with isotope dilution-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the samples were hydrolyzed by β-glucuronidase/aryl sulfatase for 12 h, the protein was precipitated with perchloric acid. The analytes were extracted with vortex mixer by acetonitrile after adjusting the pH value to nine, and then the extracts were purified using mixed adsorbent by dSPE. After the separation on a novel mixed-mode column of Poroshell 120 Phenyl-Hexyl (100 mm×2.1 mm, 4.0 μ m), the qualitative and quantitative analyses of the 26 analytes were operated by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring (MRM). The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges. The average recoveries of the 26 β-agonists ranged from 65.3% to 108.5%, and the relative standard deviations (RSDs) were 2.7%-13.3% in spiked sample at three levels. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.03-0.1 μ g/kg and 0.1-1.0 μ g/kg, respectively. The method is low cost, sensitive, reliable and suitable for the determination of residues of the 26 β-agonists in pork products.
- dispersive solid-phase extraction (dSPE),
- isotope dilution,
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- β-agonists,
- pork
1. [1]
  [1] Yue Z F. Guideline for the Detection of Veterinary Drug Residues in Food. Beijing: Standards Press of China, 2010 岳振峰. 食品中兽药残留检测指南. 北京: 中国标准出版社, 2010
2. [2]
  [2] Kuiper H A, Noordam M Y, van Dooren-Flipsen M M, et al. J Anim Sci, 1998, 76(1): 195
3. [3]
  [3] Mitchell G A, Dunnavan G. J Anim Sci, 1998, 76(1): 208
4. [4]
  [4] Hu P, Yu S W, Li H, et al. Journal of Shenzhen University Science and Engineering, 2008, 25(1): 1 胡萍, 余少文, 李红, 等. 深圳大学学报理工版, 2008, 25(1): 1
5. [5]
  [5] Zhao C. Meat Industry, 2013(12): 42 赵翀. 肉类工业, 2013(12): 42
6. [6]
  [6] Ministry of Agriculture. No. 1519 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2010-12-27) [2016-01-05]. http://www.moa.gov.cn/govpublic/XMYS/201101/P020110113359668218325.doc 农业部. 中华人民共和国农业部公告第1519号. (2010-12-27) [2016-01-05]. http://www.moa.gov.cn/govpublic/XMYS/201101/P020110113359668218325.doc
7. [7]
  [7] GB/T 22286-2008
8. [8]
  [8] Ministry of Agriculture. No. 235 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2002-12-24) [2016-01-05]. http://www.moa.gov.cn/zwllm/tzgg/gg/200302/P020050610333735313696.doc 农业部. 中华人民共和国农业部公告第235号. (2002-12-24) [2016-01-05]. http://www.moa.gov.cn/zwllm/tzgg/gg/200302/P020050610333735313696.doc
9. [9]
  [9] Wang S, Li X F, Sheng W, et al. Journal of Instrumental Analysis, 2010, 29(3): 215 王硕, 李细芬, 生威, 等. 分析测试学报, 2010, 29(3): 215
10. [10]
  [10] Chen X F, Li R F, Liu S Z. Chinese Journal of Analytical Chemistry, 2013, 41(6): 940 陈小锋, 李瑞芳, 刘曙照. 分析化学, 2013, 41(6): 940
11. [11]
  [11] Cao B, He G, Yang H, et al. Talanta, 2013, 115: 624
12. [12]
  [12] Xie W P, Huang Y Y, Hu G L. Chinese Journal of Chromatography, 2003, 21(2): 192 谢维平, 黄盈煜, 胡桂莲. 色谱, 2003, 21(2): 192
13. [13]
  [13] Rashid B A, Kwasowski P, Stevenson D. J Pharm Biomed Anal, 1999, 21(3): 635
14. [14]
  [14] Zang L N, Zhan S X, Sun S H, et al. Chinese Journal of Health Laboratory Technology, 2012, 22(5): 1006 臧李纳, 湛社霞, 孙世宏, 等. 中国卫生检验杂志, 2012, 22(5): 1006
15. [15]
  [15] Liu B, Yan H, Qiao F, et al. J Chromatogr B, 2011, 879(1): 90
16. [16]
  [16] Kong Y, Qiu Y M, Li P, et al. Journal of Instrumental Analysis, 2006, 25(2): 63 孔莹, 邱月明, 李鹏, 等. 分析测试学报, 2006, 25(2): 63
17. [17]
  [17] Wu P G, Chen H H, Wang Q, et al. Chinese Journal of Chromatography, 2008, 26(1): 39 吴平谷, 陈慧华, 王强, 等. 色谱, 2008, 26(1): 39
18. [18]
  [18] Zhu Y L, Shao D J. Chinese Journal of Veterinary Drug, 2006, 40(11): 5 朱永林, 邵德佳. 中国兽药杂志, 2006, 40(11): 5
19. [19]
  [19] Liu J, Xie Y F, Ren D D, et al. Chinese Journal of Analytical Chemistry, 2015, 42(10): 1486 刘佳, 谢云峰, 任丹丹, 等. 分析化学, 2015, 42(10): 1486
20. [20]
  [20] Liu C, Ling W, Xu W, et al. J AOAC Int, 2011, 94(2): 420
21. [21]
  [21] Lu L L, Wang Y, Hao J Y, et al. Journal of Instrumental Analysis, 2012, 31(5): 535 鲁立良, 王远, 郝家勇, 等. 分析测试学报, 2012, 31(5): 535
22. [22]
  [22] Lu J, Che W J, Zhang Y, et al. Chinese Food Science, 2012, 33(24): 311 卢剑, 车文军, 张岩, 等. 食品科学, 2012, 33(24): 311
23. [23]
  [23] Zhang X L, Luo Y J, Jiang J, et al. Chinese Journal of Chromatography, 2015, 33(8): 838 张学亮, 罗云敬, 姜洁, 等. 色谱, 2015, 33(8): 838
24. [24]
  [24] Xiong L, Gao Y Q, Li W H, et al. Meat Sci, 2015, 105: 96
25. [25]
  [25] European Commission. 2002/657/EC. (2002-08-17) [2016-01-05]. http://eur-lex.europa.eu/legal-content/EN/ALL/?uri=CELEX:32002D0657
26. [26]
  [26] van Eeckhaut A, Lanckmans K, Sarre S, et al. J Chromatogr B, 2009, 877(23): 2198
27. [27]
  [27] González-Antuña A, Domínguez-Romero J C, García-Reyes J F, et al. J Chromatogr A, 2013, 1288: 40
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