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| Simultaneous Determination of Tetracyclines and Their Degradation Products in Complicated Matrix by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry |
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| KeyWord:tetracycline antibiotics；degradation products；ultraperformance liquid chromatography with tandem mass spectrometry（ＵＰＬＣ－ＭＳ/ＭＳ） |
| Author Name | Affiliation | | WU Xiao-feng | Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China
China National Environmental Monitoring Centre, Beijing 100012, China | | ZHENG Jia-xi | Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China | | WEI Yuan-song | Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China | | ZHAO Xin | Chinese Academy of Inspection and Quarantine, Beijing 100123, China | | ZHONG Wei-ke | Chinese Academy of Inspection and Quarantine, Beijing 100123, China |
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| Abstract: |
| An analytical method was developed to simultaneously determine the three tetracyclines[tetracycline（ＴＣ）, oxytetracycline（ＯＴＣ）and chlrotetracycline（ＣＴＣ）] and their degradation products in complicated matrix, which consisted of swine manure and mushroom residues used for composting, using ultra performance liquid chromatography with tandem mass spectrometry（UPLC-MS/MS）. Samples were extracted by Na2EDTA-McIlvaine buffer at pH 4 in combination with acetonitrile and then purified through solid phase extraction. The separation was performed on UPLC column using acetonitrile and 0.1% formic acid as mobile phase. Qualitative and quantitative analysis were carried out by a triple quadrupole mass spectrometer equipped with an electrospray ionization source that operated in the positive ionization mode（ＥＳＩ＋）. All the three tetracyclines and their degradation products achieved complete separation within 7 min and the total running time was 12 min. Accompanying with a pleasant reproducibility（n=11, RSD<15%）, the linearity of calibration curve was rather good in the range of 0~6 mg·kg-1 DW（ｄｒｙ ｗｅｉｇｈｔ）, with the R2 all above 0.996 0. The recoveries of TC, OTC and CTC were 71%~89%、66%~94% and 66%~84%, respectively, at the three spiked levels of 0.2 mg·kg-1 DW, 1 mg·kg-1 DW and 4 mg·kg-1 DW. The recovery of demeclocycline was in the range of 52%~64%, and for the epimers, the recovery varied between 32% and 51% while the anhydro~tetracyclines and their corresponding epimers showed poor recoveries below 30%. The limit of detection and quantitation for the three tetracyclines and their degradation products were in the range of 1.668~17.270 μg·kg-1 and 5.561~45.918 μg·kg-1, indicating a high sensitivity for this method. Samples taken from an open windrow composting plant located in Beijing were determined by this method and the results presented that the concentrations of TC, OTC and CTC were 0.4 mg·kg-1, 1.6 mg·kg-1 and 2.9 mg·kg-1, respectively. The detected degradation products were predominately their epimers, of which epi-chlortetracycline（ＥＣＴＣ） showed a highest concentration of 2.7 mg·kg-1, closing to its parent compound CTC. Other degradation products were also found at different levels. |
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