Citation: YU Peiyao, CHEN Chuansheng, LIU Hanbing, DENG Yanling, XUE Nandong. Simultaneous determination of tetracyclines, fluoroquinolones, and sulfonamides in chicken manure using solid-phase extraction and high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2019, 37(5): 518-524. doi: 10.3724/SP.J.1123.2018.11006 shu

Simultaneous determination of tetracyclines, fluoroquinolones, and sulfonamides in chicken manure using solid-phase extraction and high performance liquid chromatography

1.
College of Environmental Science and Engineering, Central South University of Forestry and Technology, Changsha 410000, China;
2.
Institute of Soil and Solid Waste, Chinese Research Academy of Environmental Sciences, Beijing 100012, China

Received Date: 8 November 2018

Fund Project: National key Research and Development Plan (Nos. 2017YFD0800700, 2016YFD0800202).

A highly efficient and economic method for the simultaneous determination of six common antibiotics (two tetracyclines, two quinolones, and two sulfonamides) in chicken manure was developed by using solid-phase extraction and high performance liquid chromatography (SPE-HPLC). The samples were extracted by using a mixture of the EDTA-McIlvaine buffer and a mixed organic extractant (methanol-acetonitrile-acetone, 2:2:1, v/v/v), cleaned by a hydrophile-lipophile balance (HLB) cartridge, eluted by methanol-dichloromethane (7:3, v/v), and separated by HPLC with an acetonitrile-0.7% (v/v) H₃PO₄ aqueous solution as the mobile phase. The detection wavelength and temperature of the chromatographic column were 270 nm and 32℃, respectively. All antibiotics showed great linear relationships in the range of 0.5-100 mg/L; the correlation coefficients (r²) of the standard curves were between 0.9999 and 1; the recoveries of antibiotics were between 70.0% and 116.3%; and the relative standard deviations were between 1.2% and 16.6%. The limits of detection were 1.3-6.7 μg/kg; and the limits of quantity were 3.5-9.2 μg/kg. This method was used to detect antibiotics in chicken manure from a hennery in Fushun, Liaoning Province. The contents of norfloxacin and enrofloxacin (quinolones) were from not detected to 9.23 mg/kg and 1.57-7.69 mg/kg, respectively, that of sulfamethazine (sulfonamides) were 2.02-13.05 mg/kg, while sulfamethoxazole, oxytetracycline, and tetracycline were undetectable.
- solid phase extraction (SPE),
- high performance liquid chromatography (HPLC),
- antibiotic,
- chicken manure
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沈阳化工大学材料科学与工程学院沈阳 110142