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
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]
  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]
  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
4. [4]
  Yaling Chen . Basic Theory and Competitive Exam Analysis of Dynamic Isotope Effect. University Chemistry, 2024, 39(8): 403-410. doi: 10.3866/PKU.DXHX202311093
5. [5]
  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
6. [6]
  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
7. [7]
  Jingzhao Cheng , Shiyu Gao , Bei Cheng , Kai Yang , Wang Wang , Shaowen Cao . 4-氨基-1H-咪唑-5-甲腈修饰供体-受体型氮化碳光催化剂的构建及其高效光催化产氢研究. Acta Physico-Chimica Sinica, 2024, 40(11): 2406026-. doi: 10.3866/PKU.WHXB202406026
8. [8]
  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
9. [9]
  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
10. [10]
  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
11. [11]
  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
12. [12]
  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
13. [13]
  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
14. [14]
  Yanan Liu , Yufei He , Dianqing Li . Preparation of Highly Dispersed LDHs-based Catalysts and Testing of Nitro Compound Reduction Performance: A Comprehensive Chemical Experiment for Research Transformation. University Chemistry, 2024, 39(8): 306-313. doi: 10.3866/PKU.DXHX202401081
15. [15]
  Zhenhua Wang , Haoyang Feng , Xiaoyang Shao , Wenru Fan . Vitamins in Solid Propellants: Controlled Synthesis of Neutral Macromolecular Bonding Agents. University Chemistry, 2025, 40(4): 1-9. doi: 10.3866/PKU.DXHX202401007
16. [16]
  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
17. [17]
  Shijie Li , Ke Rong , Xiaoqin Wang , Chuqi Shen , Fang Yang , Qinghong Zhang . Design of Carbon Quantum Dots/CdS/Ta₃N₅ S-Scheme Heterojunction Nanofibers for Efficient Photocatalytic Antibiotic Removal. Acta Physico-Chimica Sinica, 2024, 40(12): 2403005-. doi: 10.3866/PKU.WHXB202403005
18. [18]
  Aoyu Huang , Jun Xu , Yu Huang , Gui Chu , Mao Wang , Lili Wang , Yongqi Sun , Zhen Jiang , Xiaobo Zhu . Tailoring Electrode-Electrolyte Interfaces via a Simple Slurry Additive for Stable High-Voltage Lithium-Ion Batteries. Acta Physico-Chimica Sinica, 2025, 41(4): 100037-. doi: 10.3866/PKU.WHXB202408007
19. [19]
  Asif Hassan Raza , Shumail Farhan , Zhixian Yu , Yan Wu . 用于高效制氢的双S型ZnS/ZnO/CdS异质结构光催化剂. Acta Physico-Chimica Sinica, 2024, 40(11): 2406020-. doi: 10.3866/PKU.WHXB202406020
20. [20]
  Qingqing SHEN , Xiangbowen DU , Kaicheng QIAN , Zhikang JIN , Zheng FANG , Tong WEI , Renhong LI . Self-supporting Cu/α-FeOOH/foam nickel composite catalyst for efficient hydrogen production by coupling methanol oxidation and water electrolysis. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1953-1964. doi: 10.11862/CJIC.20240028

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(196)
HTML views(4)

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