氣相層析質譜法分析尿液中之潘他唑新   全文下載

Determination of Pentazocine in Urine by Gas Chromatography-Mass Spectrometry

本研究建立一個利用選擇性離子監測方式的氣相層析質譜法以定量尿液中之潘他唑新，並應用於實驗室共同研究。研究以dextromethorphan為內標準品，經固相萃取後再以BSTFA-1%TMCS進行衍生，之後以氣相層析質譜法進行分析。本方法之線性範圍為125~1500 ng/mL（r2 = 0.997），定量極限及偵測極限分別為125及62.5 ng/mL；同日間之精確度及精密度分別為-6.3~4.7%及3.8~11.2%，而異日間之精確度及精密度則分別為-7.5~7.0%及6.2~10.0%，這些數值顯示本方法對分析尿液中潘他唑新是適用的。將所建立的方法依據國際分析化學家協會所建議之方式進行實驗室共同研究，共有9家台灣之濫用藥物尿液檢驗實驗室參與分析3組二重複的檢體，各實驗室間尿液中潘他唑新的RSDr及RSDR分別為3.0~5.2%與6.8~10.3%，其HORRAT值介於1.1~1.5，此數值顯示本分析方法在各濫用藥物尿液檢驗實驗室間具良好之再現性，未來可作為台灣的檢驗實驗室之分析參考。

A sensitive and specific gas chromatography-mass spectrometry (GC-MS) method using selected ion monitoring (SIM) has been developed for quantification of pentazocine in urine. This method uses solid-solid extraction (SPE) and N, O-bis (trimethylsilyl) trifluoroacetamide with 1% trimethylchlorosilane derivatization, followed by GC-MS analysis using dextromethorphan as the internal standard. The method was linear between 125 and 1500 ng/mL (r2 = 0.997). The limit of quantification and limit of detection were 125 and 62.5 ng/mL, respectively. The intraday accuracy and precision were -6.3~4.7% and 3.6~11.2%, respectively. The interday accuracy and precision were -7.5~7.0% and 6.2~10.0%, respectively. These data showed that the GC-MS method was suitable for the determination of pentazocine in urine. This method was further applied to an interlaboratory study. The collaborative study was given by the Association of Official Analytical Chemists International (AOAC International). Nine drug abuse urine testing laboratories in Taiwan participated to analyze 3 samples in duplicate. The repeatability relative standard deviation (RSDr) and reproducibility relative standard deviation (RSDR) values were 3.0~5.2% and 6.8~10.3%, respectively. The method showed acceptable reproducibility, as evidenced by HORRAT values of 1.1 to 1.5. The method recommended for use by the drug abuse urine testing laboratories in Taiwan.