Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.
A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.
Tagiri-Endo
Misako
M
Institute of Public Health and Environment, Miyagi Prefectural Government, 4-7-2 Saiwai-cho, Miyagino-ku, Sendai, 983-8666, Japan. endo-mi592@pref.miyagi.jp
Suzuki
Shigeru
S
Nakamura
Tomoyuki
T
Hatakeyama
Takashi
T
Kawamukai
Kazuo
K
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008297:Male; D015203:Reproducibility of Results; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D000900:Anti-Bacterial Agents; D014874:Water Pollutants, Chemical