Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16712
標題: 液相層析串聯質譜術與高場不對稱波離子移動能譜術於尿液中濫用藥物之分析
Application of Liquid Chromatography-Tandem Mass Spectrometry and High-Field Asymmetric-Waveform Ion Mobility Spectrometry for Analyzing of Abused Drugs in Urine
作者: 陳崇宇
Chen, Chung-Yu
關鍵字: Mass spectrometry
質譜術
Abused drug
FAIMS
濫用藥物
高場不對稱波離子移動能譜術
出版社: 化學系所
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摘要: 本研究主要是利用液相層析串聯質譜技術與高場不對稱波離子移動能譜術於尿液中濫用藥物之分析。尿液經由一孔徑為0.2 μm注射針過濾器(syringe filter)過濾後,直接注入液相層析質譜儀進行分析。利用5公分短液相層析管柱與合適的層析沖提條件,分離尿液中十九種不同類型之濫用藥物後,再以加熱式電灑游離法正離子模式,將分析物從液相轉變成氣態離子,最後使用串聯質譜技術中選擇反應偵測模式進行分析。在最佳的游離化與離子傳送條件下,對於尿液中濫用藥物偵測極限低於8.4 ng/mL,線性範圍為0.5 ~ 900 ng/mL。針對尿液中不同濃度之濫用藥物分析精密度均低於24.6 %。應用此方法於真實尿液樣品之分析,可測得濫用藥物使用者尿液中安非他命類(AM與MA)濃度為118 ~ 1721 ng/mL;安非他命衍生物類 (MDA與MDMA)濃度為338 ~ 86341 ng/mL;美沙東濃度為396 ng/mL;嗎啡濃度為917 ~ 2467 ng/mL;愷它命類(K、NK與DHNK)濃度為 727 ~ 20297 ng/mL;118 ~ 1721 ng/mL。 研究亦對於高場不對稱波離子移動能譜術之原理進行簡單的介紹,實驗探討酪胺酸類化合物,於高場不對稱波離子移動能譜術中相關參數進行最佳化之探討。使用高場不對稱波離子移動能譜儀分析酪胺酸類化合物,在分散電壓為-4500 V;含有40 %氦氣之載流氣體 (carrier gas)流速為3 L/min;內/外電極溫度為80/100 ºC的條件下有最佳的分離條件與訊號強度。在最佳分析條件下,於水溶液與血清中酪胺酸化合物含量進行分析,可測得在水中酪胺酸之定量範圍為0.25 ~ 10 μg/mL,於血清基質中之定量範圍為 2 ~ 20 μg/mL。 研究最後結合高場不對稱波離子移動能譜術與液相層析串聯質譜術於尿液中愷他命與其代謝物分析之研究進行探討。在分散電壓為-4500 V;含有40 %氦氣之載流氣體 (carrier gas)流速為3 L/min;內/外電極溫度為80/100 ºC的條件下,高場不對稱波形離子移動能譜術分析愷它命及其代謝物有最佳之離子分離與穿透效果。在此最佳條件下,固定補償電壓為-5.5 V,結合液相層析串聯質譜術直接分析尿液中愷它命之含量,所得之線性範圍在0.5 ~ 500 ng/mL之間。相較於液相層析串聯質譜術,所開發方法分析尿液中愷它命類化合物可得到較高之訊號-雜訊比,因此具有較低之分析偵測極限。
This research is concerned with the development of two analytical methods, liquid chromatography-heated electrospray ionization-tandem mass spectrometry (LC-HESI-MS/MS) and high-field asymmetric waveform ion mobility spectrometry (FAIMS), for analyzing various abused drugs in urine and tyrosine in water and serum. For LC-HESI-MS/MS, chromatographic analysis was performed on a short (5 cm) C18 reverse phase column using a linear gradient of 10 mM ammonium acetate containing 0.1 % formic acid-methanol as mobile phase, total analytical time was 7 minutes. A simple sample preparation method was used by passing urine sample through a 0.22 μm syringe filter. The detection limits of target abused drugs analyzed by proposed method were ranged from 0.03 ng/mL (cocaine) to 8.4 ng/mL (morphine); the linear range was from 0.5 to 900 ng/mL with relative standard deviation value below 16.5 % (intra-day precision) and 24.6 % (inter-day precision). The feasibility of applying the proposed method to determine various abused drugs in real samples was examined by analyzing urine samples form drug-abused suspects. The abused drugs including ketamines and amphetamines were detected in suspected urines. The results demonstrate the suitability of LC-HESI-MS/MS for high throughput screening of the various abused drugs in urine. Second investigation evaluates FAIMS-MS to analyze tyrosines including (Tyr)、(Tyr)3 and (Tyr)6. Under the optimal FAIMS conditions: DV: -4500 V; carrier gas composition: 40 % He in N2;carrier gas flow rate : 3 L/min; inner/outer electrode temperature: 80/100 ºC, analyzing tyrosines by FAIMS-MS has maximum ion separation and transmission efficiency. For analyzing of tyrosine in water solution and serum by FAIMS-MS/MS, the linearity range is from 0.25 to 10 and 2 to 20 μg/mL, respectively. In third investigation, FAIMS combined with LC-MS/MS was used to analyzing ketamine, norketamine and dehydronorketamine in urine. For FAIMS analyzing, ketamine and its metabolits has maximum ion separation and transmission efficiency under the optimal FAIMS conditions, DV: -4700 V; carrier gas composition: 20 % He in N2;carrier gas flow rate : 3 L/min; inner/outer electrode temperature: 70/90 ºC. For LC-FAIMS-MS/MS analyzing, the CV was set at -5.5 V for ketamine and its metabolites. Without any sample preparation process, urine sample was directly injected and analyzed by proposed method. The linearity range was from 0.5 to 500 ng/mL and the detection limits and qutification limits were range from 0.01 ~ 0.08 ng/mL and 0.03 ~ 0.26 ng/mL, respectively. Comparing LC-FAIMS-MS/MS and LC-MS/MS methods for analyzing ketamines in urine, the LC-FAIMS-MS/MS has higher signal-to-noise ratio than LC-MS/MS due to the reduction of noise.
URI: http://hdl.handle.net/11455/16712
其他識別: U0005-0707200917263400
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