Citation: WU Dan, HAN Mei-Lin, ZOU De-Xun, WANG Xu-Ming, GAO Min, QIU Tian-Lei. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of 16 Kinds of Residual Antibiotics in Chicken Manure[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(9): 1389-1396. doi: 10.11895/j.issn.0253-3820.170173 shu

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of 16 Kinds of Residual Antibiotics in Chicken Manure

WU Dan ^1,2, ,
HAN Mei-Lin ² ,
ZOU De-Xun ¹ ,
WANG Xu-Ming ² ,
GAO Min ² ,
QIU Tian-Lei ²

1.
Department of Environmental Science and Engineering, Beijing University of Chemical Technology, Beijing 10029, China;2 Beijing Agro-Biotechnology Research Center, Beijing Academy of Agriculture and Forestry Sciences, Beijing 100097, China

Received Date: 20 March 2017
Revised Date: 24 June 2017

Fund Project: This work was supported by the Natural Science Foundation of Beijing, China (No.BAIC04-2017), the National Science and Technology Major Project of the Ministry of Science and Technology of China (No.2016YFD0800205), Key Research and Development Plan of Ministry of Science and Technology of China(No. 2017YFD0801402)and National Natural Science Foundation of China(No. 51308022).

A sensitive and effective method for determination of 16 kinds of antibiotics, including tetracycline, sulfonamide, fluoroquinolone and macrolide, in livestock and poultry manure using solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. Aiming at the chemical properties and sample impurities of the target, the parameters such as mass spectrum conditions, types of extraction and ultrasonic power were optimized. Finally, the samples were extracted with 50% acetonitrile in phosphate buffer solution (pH=4) for three times, followed by ultrasonic steaming, centrifugal and rotary, dilution, and purified by SAX-HLB. After sample loading, the solid phase was washed with 10 mL of methanol-acetone (80:20, V/V), evaporated to near dryness at 35℃, and then re-dissolved and vortex mixed in 1 mL of 0.1% formic acid:methanol (1:1, V/V). The extracts were analyzed with UPLC-MS/MS and calculated by external standard method based on the monitored product ion. The results indicated that the average spiked recoveries of tetracycline, sulfonamide, fluoroquinolone and macrolide in manure were 56.4%-94.6% with relative standard deviations (RSDs) of 2.6%-19.8%, the LODs (S/N=3) were 0.01-2.50 μg/kg, and the LOQs (S/N=10) were 0.05-7.90 μg/kg. The method was simple with high stability, high sensitivity and good reproducibility, and suitable for the simultaneously determination of many antibiotics in animal and poultry manure.
- Tetracycline,
- Sulfonamide,
- Fluoroquinolone,
- Macrolide,
- Solid-phase extraction,
- Ultra performance liquid chromatography-tandem mass spectrometry,
- Animal and poultry manure
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