Determination of Nine Polypeptide Antibiotics Residues in Animal Tissue Food by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

LI Lianwei; YANG Xiaocong; YAO Minna; LIU Zhengcai; LI Xiaojing

doi:10.13386/j.issn1002-0306.2021120013

Volume 43 Issue 17

Aug. 2022

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Science and Technology of Food Industry > 2022 > 43(17): 330-337. > DOI: 10.13386/j.issn1002-0306.2021120013

LI Lianwei, YANG Xiaocong, YAO Minna, et al. Determination of Nine Polypeptide Antibiotics Residues in Animal Tissue Food by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(17): 330−337. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021120013.

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Determination of Nine Polypeptide Antibiotics Residues in Animal Tissue Food by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

1.
Food Science College of Fujian Agriculture and Forestry University, Fuzhou 350002, China
2.
Food College of Xinyang College of Agriculture and Forestry, Xinyang 464000, China
3.
Technology Center of Fuzhou Customs District, Fuzhou 350001, China

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Received Date: December 01, 2021
Available Online: June 28, 2022

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Abstract

Abstract

A method combining SPE and Ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) was developed for the simultaneous determination of nine polypeptide antibiotics in animal tissues. The samples were extracted by methanol and 0.1 mol/L hydrochloric acid (7:3, v/v), then cleaned with Alumina-A and n-hexane, and finally purified by hydrophilic-lipophilic balance (hydrophilic-lipophilic balance, HLB) cartridge. The separations were performed on a C₈ column (100A, 150 mm×2 mm, 3 µm) using a mobile phase gradient with 0.2% formic acid and acetonitrile. Electrospray positive ionization and multi-reaction monitoring (MRM) mode were used for detection. The calibration curves for vancomycin, norvancomycin, enramycin A, enramycin B, and teicoplanin, (concentration range 2~200 μg/L), colistin A, colistin B and bacitracin A (concentration range 5~500 μg/L), virginiamycin M1 (concentration range 0.1~20 μg/L) were linear with correlation coefficients more than 0.99. The limits of quantification (LOQ, S/N=10) of 9 kinds of polypeptide antibiotics were varied from 1 µg/kg to 20 µg/kg, the detection limit of the method was 0.3 µg/kg to 6 µg/kg. The recovery experiments were performed with chicken, pork, liver and kidney samples spiked in the range of 1~200 μg/kg. The average recoveries ranged from 74.2% and 96.3% with the relative standard deviations (RSDs) of 4.3%~14.6% (n=6). The method is simple and rapid with high sensitivity and good reproducibility. Furthermore, this method is effective for the safety monitoring of polypeptide antibiotic residues in animal tissues.

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