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Sensitive Determination of Four Polypeptide Antibiotic Residues in Milk Powder by High Performance Liquid Chromatography–Electrospray Tandem Mass Spectrometry

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Abstract

Polypeptide antibiotics abuse can lead to antibiotic residues in food products and have unwanted effects on human health. A selective, accurate, and sensitive analytical method for the simultaneous determination of four polypeptide antibiotics (gramicidin S, bacitracin, polymyxin B, and polymyxin E) in infant formula powder was developed using solid-phase extraction (SPE) combined with high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). The samples were extracted with acidified methanol, deproteinized with acetonitrile, and degreased with n-hexane before SPE. After cleanup with 0.1% formic acid and methanol (3:1, v/v) in Oasis HLB cartridges, the extracts were analyzed by HPLC–MS/MS with electrospray ionization (ESI) source and time-scheduled multiple reaction monitoring (MRM). Linearity was assessed by using matrix-matched standard calibration and good determination coefficients (r2 > 0.995) were obtained. The average recoveries for blank sample at three spiked concentration levels were in the range of 82.8–101.2%. The limits of detection (LODs) and limits of quantitation (LOQs) of all analytes were in the range of 5–15 μg kg−1 and 20–50 μg kg−1, respectively. The intra-day and inter-day precisions were lower than 10%. The results of method validation demonstrated that the developed method is accurate and reliable, and it can be applied for screening and quantitation of target polypeptide antibiotics in food.

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Acknowledgements

The authors wish to acknowledge the financial support given by the project of National Key Research and Development Program of China and Public Welfare Fund of Inspection and Quarantine of China.

Funding

This study was funded by the project of National Key Research and Development Program of China and Public Welfare Fund of Inspection and Quarantine of China (Grant Numbers 2018YFC1603606, 201510038, 2016YFD0401103, and 2016YFF0203903).

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Author notes

  1. Tong Liu and Chuanbin Zhang contributed equally as first authors.

Authors and Affiliations

  1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing, 100176, China

    Tong Liu, Chuanbin Zhang, Feng Zhang, Fei Yuan & Hongna Li

  2. School of Chemistry and Chemical Engineering, Qingdao University, Qingdao, 266071, Shandong, China

    Chuanbin Zhang & Hailan Huang

  3. Key Laboratory of Chinese Internal Medicine of Ministry of Education and Beijing, Dongzhimen Hospital, Beijing University of Chinese Medicine, Beijing, 100700, China

    Bo Nie

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  1. Tong Liu
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Correspondence to Feng Zhang.

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Liu, T., Zhang, C., Zhang, F. et al. Sensitive Determination of Four Polypeptide Antibiotic Residues in Milk Powder by High Performance Liquid Chromatography–Electrospray Tandem Mass Spectrometry. Chromatographia 82, 1479–1487 (2019). https://doi.org/10.1007/s10337-019-03777-y

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