- 學位論文
以液相層析電噴灑四極柱飛行時間質譜儀對新興濫用藥物之分析
Determination of Designer Drugs by Liquid Chromatography/Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry (LC/ESI-Q-TOFMS)
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摘要
本實驗以液相層析/電噴灑游離四極柱飛行時間質譜儀 (liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry, LC/ESI-Q-TOFMS)對哌類、鹵素安非他命類濫用藥物進行分離與偵測；對酮胺類、苯乙胺類濫用藥物進行偵測。 利用液相層析法對哌類濫用藥物進行分離，其沖提條件為含氨水之 0.1 % 甲酸水溶液 (pH=3.3)和乙腈，總滯留時間為 18 分鐘。以 LC-Q-TOF對七種哌類濫用藥物的偵測極限 (S/N=3)為 7.5~75 ng⁄mL。真實樣品的部分，為無不良嗜好健康捐贈者的唾液檢體，將七種哌類濫用藥物額外添加至唾液檢體中，經由液液萃取對唾液檢體進行前處理，再以最佳化液相層析電噴灑四極柱飛行時間質譜儀條件對唾液檢體進行檢測，其平均萃取效率約為 80 %。並利用 LabVIEW (Laboratory Virtual Instrumentation Engineering Workbench)自 撰質譜校正程式 (index比對法與內插法)與譜峰辨識程式來提升質譜的準確度和可信度。 本實驗建立了哌類、鹵素安非他命類、酮胺類、苯乙胺類濫用藥物在電噴灑游離為正電壓模式下的特徵斷裂譜峰，以提供未來制定法規之相關毒品檢驗與防治的參考依據。
並列摘要
In this study, the optimal conditions for the separation and detection of four types of designer drugs, including piperazine, halogenamphetamine, aminoketone and phenethylamine derivatives were determined, using liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (LC-Q-TOFMS). Complete separation for 7 piperazines can be achieved within ~18 min using gradient elution (A, 0.1% formic acid aqueous solution containing ammonium hydroxide/pH=3.3; B, acetonitrile). The limit of detection (LOD at S/N = 3) obtained by LC/ESI-Q-TOFMS was range from 7.5 to 75 ng/mL. The saliva sample was obtained by spiking saliva received from volunteers with 7 piperazine derivatives. After liquid-liquid extraction, the samples were quantitatively analyzed using the LC/ESI-Q-TOFMS. The extraction procedures used for the saliva sample and the experimental conditions for the separation and detection were optimized. The average extraction efficiency of the saliva sample was 80 % approximately. To improve the precision and reliability we use a homebuilt mass calibration program and pattern recognition by means of LabVIEW (Laboratory Virtual Instrumentation Engineering Workbench). The characteristic mass fragmentations of four types of designer drugs, including piperazine, halogenamphetamine, aminoketone and phenethylamine derivatives, were investigated by means of LC/ESI-Q-TOFMS. As a result, the protonated molecular ion ([M+H]+) and the fragments were found to be characteristic and useful in the rapid screening and confirmation of four types of designer drugs.
參考文獻
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