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Se Pu. 2019 May 8;37(5):518-524. doi: 10.3724/SP.J.1123.2018.11006.

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

[Article in Chinese]

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


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.


antibiotic; chicken manure; high performance liquid chromatography (HPLC); solid phase extraction (SPE)

[Indexed for MEDLINE]

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