2008 年 18 巻 4 号 p. 511-520
A simple and sensitive method for the simultaneous determination of 15 non-steroidal antiinflammatory drugs (NSAIDs)—acetaminophen, ibuprofen, naproxen, fenoprofen, flurbiprofen, loxoprofen, ketoprofen, mefenamic acid, flufenamic acid, diclofenac, tolfenamic acid, oxaprozin, phenylbutazone, indomethacin, and acemetacin—in environmental water was developed. This method consists of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS-MS). These NSAIDs were analyzed within 10 min using an ODS-3 column and 5 mM aqueous ammonium formate/acetonitrile (60/40, v/v) as the mobile phase. Electrospray ionization conditions in the negative ion mode were optimized for MS-MS detection of these drugs. The optimum in-tube SPME conditions were 20 draw/eject cycles of 40 μL of sample at a flow rate of 150 μL/min using a Carboxen-1006 PLOT capillary column as an extraction device. The extracted NSAIDs were easily desorbed from the capillary by passage of mobile phase. Using the in-tube SPME/LC-MS-MS method, good linearity of the calibration curve (r≥0.9997) was obtained in the concentration range from 0.1∼10 ng/mL for all compounds examined. The limits of detection (S/N=3) of NSAIDs ranged from 5∼65 pg/mL. This method could be successfully applied to analysis of surface water and wastewater without any other pretreatment or interference peaks. The recoveries of NSAIDs spiked into river water were above 80%, and the relative standard deviations were below 8.3%. Among the NSAIDs tested in this study, loxoprofen was detected in hospital wastewater at 458 pg/mL.
