Simultaneous determination of tetracyclines and their degradation products in environmental waters by liquid chromatography-electrospray tandem mass spectrometry.

A sensitive method was developed for the trace determination of six tetracyclines and ten of their degradation products in influent, effluent, and river waters using liquid chromatography-electrospray tandem mass spectrometry detection, combined with Oasis hydrophilic-lipophilic balance (HLB) cartridge extraction and Oasis mixed-mode strong anion exchange (MAX) cartridge cleanup. Tetracyclines and their products were separated by liquid chromatography in 9.5min, and the instrument detection limits were generally between 0.03 and 0.1microg/L except for minocycline (0.5microg/L). The chromatograms were improved through the MAX cleanup and no apparent matrix effect was found. The recoveries of all the target compounds except for 4-epianhydrochlortetracycline and anhydrochlortetracycline (34-52%) were 75-120% for influent, 61-103% for effluent, and 64-113% for river waters. The method detection limits (MDLs) of the analytes varied in the range of 0.8-17.5ng/L in all studied matrices. The method was applied for the determination of tetracyclines and their products in a sewage treatment plant (STP) and surface waters in Beijing, China. Oxytetracycline (3.8-72.5ng/L), tetracycline (1.9-16.5ng/L), and five products including 4-epitetracycline, 4-epioxytetracycline, isochlortetracycline, anhydrotetracycline, and 4-epianhydrochlortetracycline (5.7-25.3ng/L) were detected in wastewater, while only oxytetracycline and tetracycline (2.2 and 2.1ng/L) were detected in surface water samples.