著者
根岸 祥子 中園 裕紀子 神田 康司 辻川 健治 桑山 健次 金森 達之 岩田 祐子 宮本 和奈 糟谷 史代 井上 博之
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.19, no.2, pp.111-119, 2014 (Released:2014-07-30)
参考文献数
16
被引用文献数
6 5

Methylamphetamines (methylamphetamine (Me-AP) and methylmethamphetamine (Me-MA)) have three ringpositional isomers. Among them, 4-Me-AP has been controlled as a designated substance (Shitei-Yakubutsu) in Japan since November 2012. Furthermore, Me-APs are a structural isomer of methamphetamine (MA), controlled as a stimulant. Because of the increasing number of structural isomer of designer drugs encountered in forensic science laboratories, analytical differentiation of structural isomers is a significant issue. In this study, a method for differentiation of methylamphetamines using gas chromatography/mass spectrometry (GC/MS) was developed. DB-1ms and DB-5ms columns could not separate free bases and trifluoroacetyl (TFA) derivatives of methylamphetamines while the columns incompletely separated their trimethylsilyl (TMS) derivatives. On the other hand, the mid-polar DB-17ms column separated free bases, TFA and TMS derivatives of 6 methylamphetamines though peak shapes of the free bases were tailing. The best separation was obtained from the analysis of the TMS derivatives on DB-17ms column. The mass spectra showed a little difference between the 2-, 3-Me-AP and 4-Me-AP after TFA derivatization. Also the structural isomers of Me-AP and MA could be differentiated by their EI mass spectra. The results indicated that differentiation of regioisomeric methylamphetamines could be accomplished well by GC/MS of their TMS derivatives on the mid-polar capillary column.
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

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.