本研究開發並評估-簡易的氣相層析/質譜儀方法,供定量尿中free codeine, free morphine, 6-acetylmorphine, total codeine, total morphine。抽取用之緩衝液以pH值為9.0時,其抽取回收率最高。抽取回收率,free codeine為98.3%,free morphine為76.7%,6-acetylmorPhine為85.6%,三甲基矽化衍生物在七十二小時內均非常安定,適合其定量分析。nalorphine為內標準品,以SIM (Selected Ion Monitoring)方式定量。濃度在50至1000ng/mL範圍內均具有良好的線性關係,日內及日間精密度試驗顯示,codeine的變異係數為0.47~7.72%,morphine為0.31~8.09%,6-acetylmorphine為0.49~6.15%。
A simple yet effective GCIMS protocol was developed and evaluated for the determination of free codeine, free morphine, 6-acetylmorphine, total codeine and total morphine in urine. Optimal recovery was achieved with extraction conducted at pH 9.0. Trimethylsilyl-derivatives of these analytes and the internal standard (nalorphine) were found adequately stable for a 72-hour period. Quantitative determination of the analytes was performed by selective ion monitoring. Excellent linearity was observed over the 50-1000ng/mL concentration range studied. The intraday and interday precisions range from 0.47 to 7.72% for codeine, 0.31 to 8.09% for morphine and 0.49 to 6.15% for 6-acetylmorphine. The overall recoveries for codeine, morphine and 6-acetylmorphine were found to be 98.3%, 76.7% and 85.6% respectively.