Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/90665
標題: Polypyrrole/Multi-walled Carbon Nanotube Composites Combined with Gas Chromatography-Tandem Mass Spectrometry for Determination of Ultraviolet Filters and Metabolites in Water and Urine
奈米複合材料結合氣相層析串聯質譜術於水與尿液中紫外光吸收劑及其代謝物分析之研究
作者: 廖昱甄
Yu-Chen Liao
關鍵字: ultraviolet filter
nanomaterial
gas chromatography-tandem mass spectrometer
紫外光吸收劑
奈米材料
氣相層析串聯質譜儀
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摘要: In this study, a sensitive analytical method was developed for determination of the trace ultraviolet filters (UV filters) and metabolites in water and urine samples. Polypyrrole/multi-walled carbon nanotube composites (PPy/MWCNT) was successfully synthesized, and it can be applied as sorbents for extraction combined with gas chromatography- tandem mass spectrometry. In optimum conditions, 500 μLwater at pH4 or original urine samples containing 13 ultraviolet filters was added into 1.5 mL eppendorf. Then, 200 μL PPy/MWCNT solution was added into the sample and the mixture was sonicated (560W) for 30 seconds for extraction. After centrifugation, the supernatant was removed. 125 μL ethyl acetate was added into eppendorf then sonicated (280 W) for 30 seconds. The elutent was dried under nitrogen stream and dissolved by 25 μL MSTFA. The extracts were derivatized under 200 W microwave condition for 30 seconds and then dried under nitrogen stream. After redissolved by 25 μL EA, the extracts were analysed by GC-MS/MS system. The linearity of the proposed method ranged from 0.025 to 50 ng/mL for 2OH- BP, BP-2 and BP-6; 0.0125 to 18.75 ng/mL for BP-7; 0.05 to 15 ng/mL for HBP; 0.375 to 50 ng/mL for 4-MBC; 0.025 to 25 ng/mL for BP-3; 0.0125 to 50 ng/mL for BP-1; 0.05 to 100 ng/mL for BP-8 and BP-9; 0.0125 to 25 ng/mL for OD-BAPA, OMC and BP-12 with coefficients of determination (R2) above 0.9913. The limits of detection (LODs) and limits of quantification (LOQs) were between 0.26 to 5.3 ng/L and 0.87 to 17.7 ng/L, respectively. The synthesized PPy/MWCNT material can extract analytes with high extraction efficiency and high selectivity. The proposed method can be applied to the determination of trace UV filters in water and urine samples.
本研究開發聚?咯/多層奈米碳管複合材料 (polypyrrole/ multi-walled carbon nanotube composites, PPy/MWCNT) 應用於水樣及尿液中 13 種紫外光吸收劑及其代謝物之萃取,並以微波輔助衍生化,結合氣相層析串聯質譜術之選擇反應偵測模式進行偵測之分析方法。實驗結果顯示於 500 μL pH 值調整為 4 的水樣及不調整 pH 值之尿液中,添加 200 μL 聚?咯/多層奈米碳管複合材料水溶液,以 560 W超音波震盪萃取 30 秒,可得最佳萃取效果;添加 125 μL 乙酸乙酯,於280 W超音波震盪下脫附 30 秒,可得最佳脫附效果;加入 25 μL MSTFA 衍生化試劑,並以200 W 微波輔助衍生 30 秒,可得最佳之衍生化效果。利用最佳萃取、脫附、衍生條件並於氣相層析串聯質譜偵測條件下分析水中 2OH-BP、BP-2 及 BP-6 的線性範圍為 0.025 至 50 ng/mL;BP-7 的線性範圍為 0.0125 至 18.75 ng/mL;HBP 的線性範圍為 0.05 至 15 ng/mL;4-MBC 的線性範圍為0.375至 50 ng/mL;BP-3 的線性範圍為 0.025 至 25 ng/mL;BP-1 的線性範圍為 0.0125 至 50ng/mL;BP-8 及 BP-9 的線性範圍為 0.05 至 100 ng/mL;OD-BAPA、OMC 及 BP-12 的線性範圍則為 0.0125 至 25 ng/mL,線性相關係數 (R2) 均在 0.9913 以上,偵測極限介於 0.26 到 10.6 ng/L 之間。本研究方法合成之奈米複合材料對於分析物具高選擇性且具有高萃取效率,可應用於水中及尿液中微量紫外光吸收劑之檢測參考。
URI: http://hdl.handle.net/11455/90665
文章公開時間: 10000-01-01
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