Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/14587
標題: 漩渦輔助分散式液液微萃取法結合液相層析串聯質譜術於環境水樣中非類固醇抗炎藥物之檢測
Determination of Non-Steroidal Anti-Inflammatory Drugs in Environmental Water by Vortex-Assisted Dispersive Liquid-Liquid Microextraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry
作者: 戴詩珊
Tai, Shih-Shan
關鍵字: 漩渦輔助分散式液液微萃取法
Non-Steroidal Anti-Inflammatory Drugs
液相層析串聯質譜術
環境水樣
非類固醇抗炎藥物
Environmental Water
Vortex-Assisted Dispersive Liquid-Liquid Microextraction
Liquid Chromatography-Tandem Mass Spectrometry
出版社: 化學系所
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摘要: 本研究開發一簡單且快速之漩渦輔助分散式液液微萃取結合液相層析串聯質譜術於偵測環境水樣中微量之非類固醇抗炎藥物。研究結果顯示,取經pH值調整為1之10毫升水樣置於15毫升的離心管中,添加0.75 mL丙酮和150 μL氯仿進行萃取,在3200 rpm的轉速下 vortex 1.5分鐘,再以轉速4000rpm下進行離心5分鐘。離心後,將氯仿層移至0.65毫升的微量離心管中,並利用SpeedVac離心抽乾後,以100 μL 75%的甲醇水溶液回溶,注入液相層析串聯質譜儀分析,10分鐘內,可有效分離包含ibuprofen、naproxen、mefenamic acid、fenoprofen、ketoprofen、diclofenac、indomethacin等七種非類固醇抗炎藥物與內標標準品ketoprofen-d3。所開發之分析方法對於環境水樣中之七種非類固醇抗炎藥物進行偵測,所得ibuprofen、naproxen、mefenamic acid、fenoprofen、ketoprofen、diclofenac與indomethacin之線性範圍分別為0.05-70 ng/mL、0.1-70 ng/mL、0.25-20 ng/mL、0.1-70 ng/mL、0.25-50 ng/mL、0.1-100 ng/mL與0.25-20 ng/mL,線性相關係數(R2)均在0.9945以上,偵測極限與定量極限分別介於2.5-48.6 pg/mL與8.4-162.0 pg/mL 之間。所開發方法之同日精密度與異日精密度以相對標準偏差(relative standard deviation, RSD)表示分別介於0.4-18.6% 與 3.2-19.5%之間,回收率則介於88-109%之間,其相對標準偏差於0.7-13.2%之間。所開發之方法應用於偵測環境水樣中非類固醇抗炎藥物之檢測,可測得水樣中含有0.436 ng/mL ibuprofen、0.612 ng/mL naproxen、7.888 ng/mL mefenamic acid與0.294 ng/mL diclofenac。由研究結果可得知,本研究開發分析技術可作為環境水樣中非類固醇抗炎藥物檢測方法之參考。
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.
URI: http://hdl.handle.net/11455/14587
其他識別: U0005-0808201317551800
文章連結: http://www.airitilibrary.com/Publication/alDetailedMesh1?DocID=U0005-0808201317551800
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