Title

微量固相萃取結合液相層析串聯質譜術於老鼠血清中氫氧化四甲基銨之檢測

Translated Titles

Determination of tetramethylammonium hydroxide in mouse serum by micro solid-phase extraction combined with liquid chromatography tandem mass spectrometry

Authors

林佳穎

Key Words

氫氧化四甲基銨 ; 微量固相萃取 ; 基質效應 ; 液相層析串聯質譜術 ; tetramethylammonium hydroxide ; µ ; SPE ; matrix effect ; LC-MS/MS

PublicationName

中興大學化學系所學位論文

Volume or Term/Year and Month of Publication

2011年

Academic Degree Category

碩士

Advisor

李茂榮

Content Language

繁體中文

Chinese Abstract

本研究主要是利用微量固相萃取法結合液相層析串聯質譜儀,分析老鼠血清中氫氧化四甲基銨(Tetramethylammonium hydroxide, TMAH)含量。使用混合相陽離子交換(Oasis® MCX)吸附劑之微量固相萃取管萃取血清中四甲基銨,並探討於萃取過程中沖提溶劑種類與沖提溶劑體積對萃取效果之影響,以三段四極矩液相層析串聯質譜儀之加熱式電灑游離法於正離子模式偵測四甲基銨。實驗結果顯示,利用200 µL含0.1%三氟乙酸之乙腈溶液,可得到最佳萃取效率,且僅需15 µL血清樣品即可進行分析。此技術所得相對回收率於不同濃度均高於95.6%,同日(intraday)及異日(interday)之精密度以RSD%表示均低於2.5%及9.8%,於血清中四甲基銨分析線性範圍為10~2500 ng/mL,偵測極限值(LOD)為1.9 ng/mL,定量極限值(LOQ)為6.3 ng/mL。評估基質效應對四甲基銨偵測之影響,以管柱後注入法(post−column infusion)可得基質成分在層析時間中對四甲基銨離子化效率沒有影響;以萃取後添加法(post−extraction spiked)評估基質成分於µSPE-LC-HESI-MS/MS可得基質效應(ME)為95.2%。並將此技術應用於經氫氧化四甲基銨塗覆於皮膚表面之小白鼠血清中,均可有效測得老鼠中四甲基銨濃度為1.1 µg/mL~9.1 µg/mL。

English Abstract

A simple and sensitive method using micro solid-phase extraction (µSPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination trace amount of tetramethylammonium hydroxide (TMAH) in mouse serum was evaluated in this thesis. The heated electrospray ionization (HESI) with positive mode of triple quadrupole mass spectrometry was used to analyze tetramethylammonium hydroxide. Tetramethylammonium was extracted from serum by µSPE with a mixed-mode cation exchange sorbent and 0.1% trifluoroacetic acid in acetonitrile used as the eluting solvent. The volume of sample used was 15 µL. The linear range of the method was 10-2500 ng/mL with coefficient of determination at 0.9944. The limit of detection and limit of quantitation was 1.9 and 6.3 ng/mL, respectively. The intra-day and inter-day precisions with relative standard deviations were less than 2.5 and 9.8 %, respectively. The recovery of the method was greater than 95.6 %. As the matrix effect was unconsidered from the results of post-column infusion and post-extraction spiked. The feasibility of applying the proposed method to determine tetramethylammonium in serum was examined by analyzing real mouse serum sample of TMAH-exposured. The concentration of tetramethylammonium detected was range from 1.1 µg/mL to 9.1 µg/mL. The results of this study reveal the proposed method offers low ng/mL level sensitivity and high selectivity for determination of tetramethylammonium in mouse serum.

Topic Category 基礎與應用科學 > 化學
理學院 > 化學系所
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Times Cited
  1. 蘇筠婷(2015)。分散式固相萃取技術結合高效能液相層析串聯質譜術於人體尿液中精氨酸及其衍生物之檢測。中興大學化學系所學位論文。2015。1-68。