Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (11): 998-1004.DOI: 10.3724/SP.J.1123.2022.07002

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Determination of three penicillin residues in milk by solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry using a covalent triazine framework sorbent

LI Qin1, DAI Shuyu2, YANG Yuan2, FENG Yumin2, LIAN Hongzhen3, ZHANG Shusheng2, ZHANG Wenfen2,4,*()   

  1. 1. Food and Drug Inspection Institute of Zhengzhou, Zhengzhou 450006, China
    2. College of Chemistry, Zhengzhou University, Zhengzhou 450001, China
    3. College of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China
    4. Zhengzhou Tobacco Research Institute of China National Tobacco Corporation, Zhengzhou 450001, China
  • Received:2022-07-04 Online:2022-11-08 Published:2022-11-10
  • Contact: ZHANG Wenfen
  • Supported by:
    National Natural Science Foundation of China(22004109);China Postdoctoral Science Foundation(2022M710167);Scientific and Technological Project of Administration for Market Regulation Henan Province(2022sj134)

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Abstract:

A method based on solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) was established for the determination of gpenicillin, cloxacillin, ampicillin residues in milk. Using self-made covalent triazine frameworks (CTFs) as the solid-phase extraction sorbents, the main factors influencing the efficiency of the solid-phase extraction columns, such as the sorbent amount, eluent type, eluent volume, and flow rate, were optimized. The extraction and purification conditions for the samples were also investigated. The optimal extraction effect was achieved at a flow rate of 3 mL/min with 60 mg CTFs and 6 mL eluent solution (acetonitrile). Separation was carried out on a Waters ACQUITY UPLC BEH C18 column, and 0.1% formic acid aqueous solution-acetonitrile was used as the mobile phases for gradient elution. The filtrate was detected by ultra performance liquid chromatography-tandem mass spectrometry, identified by electrospray ionization (ESI) in the positive mode using multiple reaction monitoring, and quantified using external standards. The calibration curves of the three penicillins showed good linearity and the correlation coefficients of the linear regression equations for the three target analytes were all greater than 0.999. The limits of detection (LODs) and limits of quantification (LOQs) were 0.05-0.10 μg/kg and 0.1-0.4 μg/kg, respectively. The average recoveries of the three analytes were 84.9%-94.1%, and the relative standard deviations (RSDs, n=5) were 1.66%-3.27%. Moreover, the mechanism of interaction between the CTFs and the target analytes was analyzed. The results revealed the existence of π-π and hydrogen-bond interactions between the CTFs and analytes. The results further indicated that the CTFs could be successfully used for the enrichment and purification of penicillins in milk. The proposed method has the advantages of high precision, good reproducibility, high resolution, and short analysis time, and it is suitable for the qualitative and quantitative determination of trace targets in complex matrices.

Key words: covalent triazine frameworks (CTFs), solid-phase extraction (SPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), penicillin, milk

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