著者

西岡 裕 西川 眞弓 土橋 均

出版者

日本法科学技術学会

雑誌

日本法科学技術学会誌 (ISSN:18801323)

巻号頁・発行日

vol.11, no.1, pp.53-75, 2006

被引用文献数

1

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A fully automated identification system for 35 benzodiazepines and their 29 metabolites was developed by gas chromatography-mass spectrometry (GC-MS) with a DB-5MS fused silica capillary column after trimethylsilyl (TMS) and trifluoroacetyl (TFA) derivatization, followed by registering both their retention times and mass spectra as the standard library data.<br>All the analytes except for rilmazafone and haloxazolam were detectable with and/or without TMS derivatization. TFA derivatization was found to be more effective in the more sensitive analysis of oxazolo-benzodiazepines except for flutazolam. Also, correction of their retention times by alkanes enabled to accurately identify on the different GC-MS systems with different lots of columns.<br>The present system allowed us to identify benzodiazepines and their metabolites in urine and blood more readily in a much shorter time, and it will be a powerful system for the analysis of benzodiazepines in the forensic chemistry and toxicology fields.

著者

西川 眞弓 中島 邦生 五十嵐 一雄 糟谷 史代 福井 巳芳 土橋 均

出版者

公益社団法人日本薬学会

雑誌

衛生化学 (ISSN:0013273X)

巻号頁・発行日

vol.38, no.2, pp.121-126, 1992-04-30

被引用文献数

8

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An analytical procedure for morphine-3-glucuronide (M3G) and morphine (M) in the human urine was investigated by using high-performance liquid chromatography coupled with atomospheric pressure ionization mass spectrometry (LC/APCI-MS). The samples were purified with Sep-Pak C_<18> cartridges. The LC separation was carried out using a L-column ODS in 50 mM ammonium acetate-methanol (86 : 14 v/v). The calibration graphs constructed by the absolute calibration curve method showed linearity over the concentration range of 30 to 1000 ng/ml (γ=0.9965) for M3G and 30 to 2000 ng/ml (γ=0.9970) for M. The detection limits by selected ion monitoring (SIM) were 3 ng/ml for M3G and 1 ng/ml for M, and by scan mode were 350 ng/ml for M3G and 80 ng/ml for M. The coefficients of variations for M3G and M were 4.79 and 3.15% at 1 μg/ml, respectively.