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
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