Citation: CAO Yafei, KANG Jian, CHANG Qiaoying, HU Xueyan, WANG Zhibin, FAN Chunlin, WANG Minglin. Multi-residue determination of veterinary drugs in cheese by QuEChERS and liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(2): 132-139. doi: 10.3724/SP.J.1123.2014.10022 shu

Multi-residue determination of veterinary drugs in cheese by QuEChERS and liquid chromatography- tandem mass spectrometry

CAO Yafei ^1,2 ,
KANG Jian ^2,3 ,
CHANG Qiaoying ^2,3 ,
HU Xueyan ² ,
WANG Zhibin ^2,3 ,
FAN Chunlin ^2,, ,
WANG Minglin ^1,,

1.
1. College of Food Science and Engineering, Shandong Agricultural University, Taian 271018, China;

Corresponding author: FAN Chunlin, WANG Minglin,
Received Date: 27 October 2014
Available Online: 25 November 2014
Fund Project: "十二五"国家科技支撑项目(2012BAD29B01). (2012BAD29B01)

A rapid and sensitive method has been developed for the simultaneous determination of 50 veterinary drugs (including macrolides, quinolones, sulfonamides, and tetracyclines) in cheese using a modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). After adding Na₂EDTA buffer solution and ceramic homogenizer, the cheese sample was extracted by 5% (v/v) acetic acid-acetonitrile, sodium chloride and anhydrous sodium sulfate were used for salting-out process. The resulting supernatant solution was purified by C₁₈ sorbent and the re-dissolved solution was analyzed by LC-MS/MS under dynamic multi-reaction monitoring (dynamic MRM) mode via positive electrospray ionization with a ZORBAX-SB-C₁₈ column. The limits of quantification (LOQ, S/N=10) of the target compounds ranged from 0.05 μg/kg to 20 μg/kg in cheese. At spiked levels of 20, 50, 100 μg/kg (n=6), the percentages of drug with a recovery between 70% and 120% were 94%, 92%, and 96%, respectively. The relative standard deviations (RSDs) were between 1% and 14%. This method has been applied to determine seven real samples from markets. Roxithromycin and flumequine have been detected in two samples separately. The results demonstrated that this simple, rapid and accurate method is suitable for the detection of multi-class veterinary drugs in cheese.
- QuEChERS,
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- veterinary drug,
- cheese,
- multi-residues
1. [1]
  [1] Stolker A A M, Brinkman U A T. J Chromatogr A, 2005, 1067(1/2): 15
2. [2]
  [2] Electronic Code of Federal Regulations. Tolerances for Residues of New Animal Drugs in Food. (2011-07-28) [2014-07-10]. http://ecfr.gpoaccess.gov/cgi/t/text/text-idx?c=ecfr&sid=407e94c4cd1bff327c7146f42bcc0d56&tpl=/ecfrbrowse/Title21/21cfr556_main_02.tpl
3. [3]
  [3] European Union. Commision Regulation. (2009-12-22) [2014-06-20]. http://ec.europa.eu/health/files/mrl/mrl_20101212_consol.pdf
4. [4]
  [4] The Japan Food Chemical Research Foundation. Maximum Residue Limits (MRLs) List of Agricultural Chemicals in Foods. (2011-09-30) [2014-06-21]. http://www.m5.ws001.squarestart.ne.jp/foundation/search.html
5. [5]
  [5] Ministry of Agriculture. No. 235 Bulletin of the Ministry of Agriculture of the People's Republic of China (农业部. 中华人民共和国农业部公告第235号). (2002-12-24) [2014-08-20]. http://www.moa.gov.cn/zwllm/tzgg/gg/200302/t20030226_59300.htm
6. [6]
  [6] Anastasio A, Esposito M, Amorena M, et al. J Agric Food Chem, 2002, 50 (18): 5241
7. [7]
  [7] Berardi G, Bogialli S, Curini R, et al. J Agric Food Chem, 2006, 54(13): 4537
8. [8]
  [8] Bogialli S, Coradazzi C, Di Corcia A, et al. J AOAC Int, 2007, 90(3): 864
9. [9]
  [9] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
10. [10]
  [10] Lehotay S J, Mastovska K, Yun S J. J AOAC Int, 2005, 88(2): 630
11. [11]
  [11] Lehotay S J. J AOAC Int, 2007, 90(2): 485
12. [12]
  [12] Li Y, Zheng F, Wang M L, et al. Chinese Journal of Chromatography (李岩, 郑锋, 王明林, 等. 色谱), 2009, 27(2): 127
13. [13]
  [13] Zhao Z Y, Shi Z H, Kang J, et al. Chinese Journal of Chromatography (赵志远, 石志红, 康健, 等. 色谱), 2013, 31(4): 372
14. [14]
  [14] Huang H H, Zhang J, Xu D M, et al. Chinese Journal of Chromatography (黄何何, 张缙, 徐敦明, 等. 色谱), 2014, 32(7): 707
15. [15]
  [15] Chen L, Song F, Liu Z, et al. J Chromatogr A, 2012, 1225: 132
16. [16]
  [16] Cherta L, Portoles T, Beltran J, et al. J Chromatogr A, 2013, 1314: 224
17. [17]
  [17] Stubbings G, Bigwood T. Anal Chim Acta, 2009, 637(1/2): 68
18. [18]
  [18] Aguilera-Luiz M M, Vidal J L M, Romero-Gonzalez R, et al. J Chromatogr A, 2008, 1205(1/2): 10
19. [19]
  [19] Gao F D, Zhao Y, Shao B, et al. Chinese Journal of Chromatography (高馥蝶, 赵妍, 邵兵, 等. 色谱), 2012, 30(6): 560
20. [20]
  [20] Yan X F. China Journal of Veterinary Medicine (闫小峰. 中国兽药杂志), 2010, 44(5): 47
21. [21]
  [21] Bo H B, Chen L R. Chinese Journal of Health Laboratory Technology (薄海波, 陈立仁. 中国卫生检验杂志), 2004, 14(6): 699
22. [22]
  [22] Tsai W H, Huang T C, Chen H H, et al. J Chromatogr A, 2010, 1217(3): 415
23. [23]
  [23] Taylor P J. Clin Biochem, 2005, 38(4): 328
24. [24]
  [24] Gomez Perez M L, Romero-Gonzalez R, Martinez Vidal J L, et al. J Sep Sci, 2013, 36(7): 1223
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]
  Yifan Xie , Liyun Yao , Ruolin Yang , Yuxing Cai , Yujie Jin , Ning Li . Exploration and Practice of Online and Offline Hybrid Teaching Mode in High-Performance Liquid Chromatography Experiment. University Chemistry, 2025, 40(11): 100-107. doi: 10.12461/PKU.DXHX202412133
4. [4]
  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
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]
  Qilong Fang , Yiqi Li , Jiangyihui Sheng , Quan Yuan , Jie Tan . Magical Pesticide Residue Detection Test Strips: Aptamer-based Lateral Flow Test Strips for Organophosphorus Pesticide Detection. University Chemistry, 2024, 39(5): 80-89. doi: 10.3866/PKU.DXHX202310004
7. [7]
  Xiaohong Li , Huanjiang Wang , Fang Tan , Xiaohua Cai , Yingchun Luo , Yanli Leng , Guoyong Zhou , Zhu Wen . Research on the Project-Driven Teaching Model in the Context of New Engineering: A Case Study of the Development of a “Portable Metal ions and Pesticide Residues Intelligent Detection System”. University Chemistry, 2026, 41(1): 204-212. doi: 10.12461/PKU.DXHX202510037
8. [8]
  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): 100013-0. doi: 10.3866/PKU.WHXB202309036
9. [9]
  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
10. [10]
  Xiyuan Su , Zhenlin Hu , Ye Fan , Xianyuan Liu , Xianyong Lu . Change as You Want: Multi-Responsive Superhydrophobic Intelligent Actuation Material. University Chemistry, 2024, 39(5): 228-237. doi: 10.3866/PKU.DXHX202311059
11. [11]
  Zongpei Zhang , Yanyang Li , Yanan Si , Kai Li , Shuangquan Zang . Developing a Chemistry Experiment Center Employing a Multifaceted Approach to Serve High-Quality Laboratory Education. University Chemistry, 2024, 39(7): 13-19. doi: 10.12461/PKU.DXHX202404041
12. [12]
  Ruilin Han , Xiaoqi Yan . Comparison of Multiple Function Methods for Fitting Surface Tension and Concentration Curves. University Chemistry, 2024, 39(7): 381-385. doi: 10.3866/PKU.DXHX202311023
13. [13]
  Xingyuan Lu , Yutao Yao , Junjing Gu , Peifeng Su . Energy Decomposition Analysis and Its Application in the Many-Body Effect of Water Clusters. University Chemistry, 2025, 40(3): 100-107. doi: 10.12461/PKU.DXHX202405074
14. [14]
  Weijie Yang , Mansheng Chen , Chen Xu , Fujian Xu . Hydroxyl-Rich Polycations: Innovative Materials Empowering Life and Health. University Chemistry, 2025, 40(9): 332-343. doi: 10.12461/PKU.DXHX202410072
15. [15]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
16. [16]
  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
17. [17]
  Yajie Li , Bin Chen , Yiping Wang , Hui Xing , Wei Zhao , Geng Zhang , Siqi Shi . Inhibiting Dendrite Growth by Customizing Electrolyte or Separator to Achieve Anisotropic Lithium-Ion Transport: A Phase-Field Study. Acta Physico-Chimica Sinica, 2024, 40(3): 2305053-0. doi: 10.3866/PKU.WHXB202305053
18. [18]
  Liang TANG , Jingfei NI , Kang XIAO , Xiangmei LIU . Synthesis and X-ray imaging application of lanthanide-organic complex-based scintillators. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1892-1902. doi: 10.11862/CJIC.20240139
19. [19]
  Li'na ZHONG , Jingling CHEN , Qinghua ZHAO . Synthesis of multi-responsive carbon quantum dots from green carbon sources for detection of iron ions and L-ascorbic acid. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 709-718. doi: 10.11862/CJIC.20240280
20. [20]
  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

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(708)
HTML views(112)

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