Citation: ZHANG Xiuyao, CAI Xinxin. Rapid simultaneous determination of 53 β-lactam antibiotics and their metabolites in milk by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(7): 693-701. doi: 10.3724/SP.J.1123.2014.03019 shu

Rapid simultaneous determination of 53 β-lactam antibiotics and their metabolites in milk by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry

ZHANG Xiuyao ^, ,
CAI Xinxin

1.
Wenzhou Center for Disease Control and Prevention, Wenzhou 325001, China

Corresponding author: ZHANG Xiuyao,
Received Date: 14 March 2014
Available Online: 30 April 2014
Fund Project: 温州市第三轮“311”工程建设项目基金(2008012). (2008012)

A rapid method for the determination of 53 β-lactams and their metabolites residues in milk was developed by ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). The method was based on protein precipitation by adding equal quantity of acetonitrile, followed by the ultra filtration of the extracts. The analysis of the residues was achieved on an ACQUITY BEH C₁₈ column with gradient elution using mobile phases of 0.1% formic acid in water and acetonitrile. The analytes were detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring (MRM) mode, and quantified by matrix-matched internal standard calibration. The cycle time of each analysis was 10 min. Under the optimum operation conditions, excellent linear dynamic range was observed from the quantification limits to 200 μg/kg with the correlation coefficients better than 0.9911 for all the compounds. The average recoveries for all the β-lactams and their metabolites ranged from 71% to 121% with the relative standard deviations of 1.7%-19% (n=6). This method enabled the screening for more than 50 samples per day by one person and also showed good performance for quantitation, and allowed the determination of the β-lactams and their metabolites residues in milk below the maximum residue levels (MRLs) according to the Bulletin No. 235 (2002) of Ministry of Agriculture, P. R. China and EU Regulation 2377/90/EC (2008 Revised).
1. [1]
  [1] Grunwald L, Petz M. Anal Chim Acta, 2003, 483: 73
2. [2]
  [2] Blaha J M, Knevel A M, Hem S L. J Pharm Sci, 1975, 64(8): 1384
3. [3]
  [3] Chen H, Ma W J, Tian J H, et al. Animal Husbandry and Feed Science (陈号, 马文静, 田晋红, 等. 畜牧与饲料科学), 2010, 31(1): 67
4. [4]
  [4] Tian C Q, Tan H R, Gao L P, et al. Chinese Journal of Chromatography (田春秋, 檀华蓉, 高丽萍, 等. 色谱), 2011, 29(11): 1128
5. [5]
  [5] Becker M, Zittlau E, Petz M. Anal Chim Acta, 2004, 520: 19
6. [6]
  [6] Daeseleire E, Ruyck H D, Renterghem R V. Rapid Commun Mass Spectrom, 2000, 14: 1404
7. [7]
  [7] Huang B F, Ren Y P, Cai Z X, et al. Chinese Journal of Food Hygiene (黄百芬, 任一平, 蔡增轩, 等. 中国食品卫生杂志), 2007, 19(1): 31
8. [8]
  [8] Sun L, Zhang L, Wang X, et al. Journal of Instrumental Analysis (孙雷, 张骊, 汪霞, 等. 分析测试学报), 2009, 28(5): 576
9. [9]
  [9] Qin F, Zheng W J, Chen G L, et al. Chinese Journal of Antibiotics (秦峰, 郑文捷, 陈桂良, 等. 中国抗生素杂志), 2009, 34(6): 348
10. [10]
  [10] Baere S D, Cheriet M, Baert K, et al. Anal Chem, 2002, 74: 1393
11. [11]
  [11] Li W, Ai L F, Guo C H, et al. Chinese Journal of Chromatography (李玮, 艾连峰, 郭春海, 等. 色谱), 2013, 31(10): 946
12. [12]
  [12] Chen C, Yan H, Shen B H, et al. Chinese Journal of Chromatography (陈聪, 严慧, 沈保华, 等. 色谱), 2012, 30(5): 445
13. [13]
  [13] Degelaen J P, Loukas S L, Feeney J, et al. J Chem Soc, Perkin Trans 2, 1979: 86
14. [14]
  [14] Valvo L, Alimont S, Aliment R, et al. J Pharm Biomed Anal, 1997, 15: 487
15. [15]
  [15] Ortelli D, Cognard E, Jan P, et al. J Chromatogr B, 2009, 877: 2363
1. [1]
  Junjie Zhang , Yue Wang , Qiuhan Wu , Ruquan Shen , Han Liu , Xinhua Duan . Preparation and Selective Separation of Lightweight Magnetic Molecularly Imprinted Polymers for Trace Tetracycline Detection in Milk. University Chemistry, 2024, 39(5): 251-257. doi: 10.3866/PKU.DXHX202311084
2. [2]
  Peiling Li , Qing Feng , Hongling Yuan , Qin Wang . Live Interview Recording about the Penicillin Family. University Chemistry, 2024, 39(9): 122-127. doi: 10.3866/PKU.DXHX202311022
3. [3]
  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): 2403005-0. doi: 10.3866/PKU.WHXB202403005
4. [4]
  Kexin Dong , Chuqi Shen , Ruyu Yan , Yanping Liu , Chunqiang Zhuang , Shijie Li . Integration of Plasmonic Effect and S-Scheme Heterojunction into Ag/Ag₃PO₄/C₃N₅ Photocatalyst for Boosted Photocatalytic Levofloxacin Degradation. Acta Physico-Chimica Sinica, 2024, 40(10): 2310013-0. doi: 10.3866/PKU.WHXB202310013
5. [5]
  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
6. [6]
  Chao Liu , Huan Yu , Jiaming Li , Xi Yu , Zhuangzhi Yu , Yuxi Song , Feng Zhang , Qinfang Zhang , Zhigang Zou . 具有光热效应的多级Ti₃C₂/Bi₁₂O₁₇Br₂肖特基异质结简单合成及其太阳能驱动抗生素光降解的研究. Acta Physico-Chimica Sinica, 2025, 41(7): 100075-0. doi: 10.1016/j.actphy.2025.100075
7. [7]
  Deyun Ma , Fenglan Liang , Qingquan Xue , Yanping Liu , Chunqiang Zhuang , Shijie Li . Interfacial engineering of Cd_0.5Zn_0.5S/BiOBr S-scheme heterojunction with oxygen vacancies for effective photocatalytic antibiotic removal. Acta Physico-Chimica Sinica, 2025, 41(12): 100190-0. doi: 10.1016/j.actphy.2025.100190
8. [8]
  Meijin Li , Xirong Fu , Xue Zheng , Yuhan Liu , Bao Li . The Marvel of NAD⁺: Nicotinamide Adenine Dinucleotide. University Chemistry, 2024, 39(9): 35-39. doi: 10.12461/PKU.DXHX202401027
9. [9]
  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
10. [10]
  Jijun Sun , Qianlang Wang , Qian Chen , Quanqin Zhao , Shumei Zhai . The Antibiotic Legion’s Manifesto to Human Allies. University Chemistry, 2025, 40(4): 307-321. doi: 10.12461/PKU.DXHX202405206
11. [11]
  Yongzhi LI , Han ZHANG , Gangding WANG , Yanwei SUI , Lei HOU , Yaoyu WANG . A two-dimensional metal-organic framework for the determination of nitrofurantoin and nitrofurazone in aqueous solution. Chinese Journal of Inorganic Chemistry, 2025, 41(2): 245-253. doi: 10.11862/CJIC.20240307
12. [12]
  Liangzhen Hu , Li Ni , Ziyi Liu , Xiaohui Zhang , Bo Qin , Yan Xiong . A Green Chemistry Experiment on Electrochemical Synthesis of Benzophenone. University Chemistry, 2024, 39(6): 350-356. doi: 10.3866/PKU.DXHX202312001
13. [13]
  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
14. [14]
  Qi Wu , Changhua Wang , Yingying Li , Xintong Zhang . Enhanced photocatalytic synthesis of H₂O₂ by triplet electron transfer at g-C₃N₄@BN van der Waals heterojunction interface. Acta Physico-Chimica Sinica, 2025, 41(9): 100107-0. doi: 10.1016/j.actphy.2025.100107
15. [15]
  Ran Yu , Chen Hu , Ruili Guo , Ruonan Liu , Lixing Xia , Cenyu Yang , Jianglan Shui . Catalytic Effect of H₃PW₁₂O₄₀ on Hydrogen Storage of MgH₂. Acta Physico-Chimica Sinica, 2025, 41(1): 100001-0. doi: 10.3866/PKU.WHXB202308032
16. [16]
  Jinglun Wang , Hu Zhou , Baishu Zheng , Guobin Li , Ming Yue , Zhihua Zhou . Exploration and Practice of “Four Cooperations and Four Integrations” to Cultivate Innovative Talents in Chemical Materials in Local Colleges. University Chemistry, 2024, 39(7): 93-98. doi: 10.12461/PKU.DXHX202405013
17. [17]
  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
18. [18]
  Xiaoyang Li , Xiaowei Huang , Yimeng Zhang , Huan Liu , Shao Jin , Junpeng Zhuang . Comprehensive Chemical Experiments on the Synthesis of 1,3-Dibromo-5,5-Dimethylhydantoin and Its Application as a Brominating Reagent. University Chemistry, 2025, 40(7): 286-293. doi: 10.12461/PKU.DXHX202408035
19. [19]
  Shumin Zhang , Yaqi Wang , Zelin Wang , Libo Wang , Changsheng An , Difa Xu . Ultrafast electron transfer at the ZIS_1−x/UCN S-scheme interface enables efficient H₂O₂ photosynthesis coupled with tetracycline degradation. Acta Physico-Chimica Sinica, 2025, 41(11): 100136-0. doi: 10.1016/j.actphy.2025.100136
20. [20]
  Qianqian Liu , Xing Du , Wanfei Li , Wei-Lin Dai , Bo Liu . Synergistic Effects of Internal Electric and Dipole Fields in SnNb₂O₆/Nitrogen-Enriched C₃N₅ S-Scheme Heterojunction for Boosting Photocatalytic Performance. Acta Physico-Chimica Sinica, 2024, 40(10): 2311016-0. doi: 10.3866/PKU.WHXB202311016

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(476)
HTML views(14)

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