Nakamae Takuma, Shinozuka Tatsuo, Sasaki Chizuko, Ogamo Akira, Murakami-Hashimoto Chikako, Irie Wataru, Terada Masaru, Nakamura Shigeki, Furukawa Masataka, Kurihara Katsuyoshi
Department of Pharmaceutical Science, International University of Health and Welfare, 2600-1 Kitakanemaru, Ohtawara, Tochigi 324-8501, Japan.
Forensic Sci Int. 2008 Nov 20;182(1-3):e1-6. doi: 10.1016/j.forsciint.2008.08.012. Epub 2008 Oct 30.
A simultaneous analytical method for etizolam and its main metabolites (alpha-hydroxyetizolam and 8-hydroxyetizolam) in whole blood was developed using solid-phase extraction, TMS derivatization and ion trap gas chromatography tandem mass spectrometry (GC-MS/MS). Separation of etizolam, TMS derivatives of alpha-hydroxyetizolam and 8-hydroxyetizolam and fludiazepam as internal standard was performed within about 17 min. The inter-day precision evaluated at the concentration of 50 ng/mL etizolam, alpha-hydroxyetizolam and 8-hydroxyetizolam was evaluated 8.6, 6.4 and 8.0% respectively. Linearity occurred over the range in 5-50 ng/mL. This method is satisfactory for clinical and forensic purposes. This method was applied to two unnatural death cases suspected to involve etizolam. Etizolam and its two metabolites were detected in these cases.
采用固相萃取、TMS衍生化和离子阱气相色谱串联质谱法(GC-MS/MS)建立了全血中依替唑仑及其主要代谢物(α-羟基依替唑仑和8-羟基依替唑仑)的同步分析方法。依替唑仑、α-羟基依替唑仑和8-羟基依替唑仑的TMS衍生物以及作为内标的氟硝西泮在约17分钟内实现分离。在依替唑仑、α-羟基依替唑仑和8-羟基依替唑仑浓度为50 ng/mL时评估的日间精密度分别为8.6%、6.4%和8.0%。线性范围为5-50 ng/mL。该方法用于临床和法医目的令人满意。该方法应用于两起疑似涉及依替唑仑的非自然死亡案件。在这些案件中检测到了依替唑仑及其两种代谢物。