| Summary: | 碩士 === 國立中興大學 === 化學系所 === 101 === In this study, the vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed to detect trace non-steroidal anti-inflammatory drugs (NSAIDs) in the environmental water samples. In this research, an aliquot of 10 mL water sample pH adjusted of 1 was placed in a 15 mL centrifuging tube and subsequently added 0.75 mL of acetone and 150 μL of chloroform in the same tube. The mixed solution was vortexed at 3200 rpm for 1.5 min and then centrifuged at 4000 rpm for 5 min. After centrifuging, the chloroform layer was removed to a 0.65 mL eppendorf and evaporated to dryness by SpeedVac. The residue was dissolved with 100 μL 75% methanol aqueous solution and the solution reconstructed was injected into the LC-MS/MS for analysis. The target non-steroidal anti-inflammatory drugs including ibuprofen, naproxen, mefenamic acid, fenoprofen, ketoprofen, diclofenac, indomethacin and internal standard ketoprofen-d3, were successfully separated by LC-MS/MS in 10 minutes The linearities of proposed method were 0.05-70 ng/mL for ibuprofen, 0.1-70 ng/mL for naproxen, 0.25-20 ng/mL for mefenamic acid, 0.1-70 ng/mL for fenoprofen, 0.25-50 ng/mL for ketoprofen, 0.1-100 ng/mL for diclofenac, and 0.25-20 ng/mL for indomethacin and the coefficients of determination (R2) were above 0.9945. The limits of detection (LODs) and limits of quantitation (LOQs) were 2.5-48.6 pg/mL and 8.4-162.0 pg/mL, respectively. The intra-day and inter-day precisions expressed with relative standard deviation (RSD) were 0.4-18.6% and 3.2-19.5%, respectively. The recoveries of the method proposed ranged from 88 to 109% with relative standard deviation between 0.7% and 13.2%. The method proposed was tested by analyzing trace non-steroidal anti-inflammatory drugs residues in environmental water samples of Taichung area and the results showed the trace of non-steroidal anti-inflammatory drugs were detected in the range of 0.294-7.888 ng/mL. The results demonstrate the adequacy of the VA-DLLME-LC-MS/MS method for determination of trace non-steroidal anti-inflammatory drugs in environmental water samples.
|
|---|
