著者

浅井 龍太郎 鎌田 徹 新田 篤志 和田 美暁 掛橋 秀直 中野 史保子 松田 駿太朗 志摩 典明 西岡 裕 三木 昭宏 片木 宗弘

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.24, no.1, pp.43-48, 2019 (Released:2019-01-31)

参考文献数

18

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In order to expose substituted, cheated and faked urine specimens submitted for a drug test, a simple and highly sensitive screening method has been developed for the detection of urea in the specimens. This method uses the coloration of a piece of pH test paper which is wetted and set into the headspace of a sample vial containing “urine”, by absorbing NH3 gas generated by the urease reaction. The present method named, “Urease-Headspace method” (UHS method), was evaluated by applying it to various diluted or adulterated urine samples. The detection limit of urea in water was 2×10−4%, which was 100 times higher sensitivity compared with a conventional p-(dimethylamino)cinnamaldehyde (DAC) test. The UHS method was applicable even to deeply colored specimens such as bloody urine because the coloration occurs in the headspace of the sample vial. The UHS method quickly revealed the substituted specimens, e.g. water and green tea. Thus, the present UHS method will be effective for the validity determination of urine specimens, which is increasingly crucial in forensic drug examination.

著者

松田 駿太朗 掛橋 秀直 中野 史保子 志摩 典明 鎌田 徹 西岡 裕 三木 昭宏 坂本 雄紀 宮川 治彦 草野 麻衣子 財津 桂 土橋 均 片木 宗弘

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.22, no.2, pp.109-121, 2017 (Released:2017-07-27)

参考文献数

13

被引用文献数

3

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In this study, we describe a rapid gas chromatography-tandem mass spectrometry (GC-MS/MS) analytical method that allows comprehensive detection and structural elucidation of synthetic cathinone-type designer drugs. Our proposed method consists of three simultaneous analytical procedures: 1) selective detection of the carbonyl group characteristic to each cathinone examined via selected reaction monitoring (SRM); and the determination of both 2) iminium cations and 3) substituted benzoyl cations generated via the α-cleavage of their corresponding amines and ketone moieties via product ion scanning, respectively.  One peak was detected in the SRM chromatogram for all cathinones examined in procedure 1), as well as the relevant single peaks in the total ion current chromatograms that resulted from procedures 2) and 3) at the same retention time. SRM of procedure 1) showed the transition of substituted benzoyl cations to substituted phenyl cations due to CO elimination, revealing the presence of carbonyl groups within the structures. Each product ion spectrum of the substituted benzoyl cation allowed for both determination of which group was substituted on the aromatic ring and differentiation between corresponding positional isomers for ethyl, methoxy and methylenedioxy substitution. However, identification of the substitution positions for the methyl, bromine and fluorine groups on the aromatic ring was difficult. On the other hand, differences between structural isomers in the product ion spectra of iminium cations were clearly identifiable, allowing for easy discrimination between isomers.

著者

掛橋 秀直 志摩 典明 鎌田 寛恵 松田 駿太朗 中野 史保子 和田 美暁 佐々木 啓子 鎌田 徹 西岡 裕 財津 桂 土橋 均 三木 昭宏 片木 宗弘

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.22, no.2, pp.77-90, 2017 (Released:2017-07-27)

参考文献数

26

被引用文献数

1

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Three analogues of 1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one (α-PVP), 1-(4-fluorophenyl)-2-(pyrolidin-1-yl)pentan-1-one (4F-α-PVP), 1-(4-methoxyphenyl)-2-(pyrrolidin-1-yl)pentan-1-one (4MeO-α-PVP) and 2-(pyrrolidin-1-yl)-1-(thiophen-2-yl)pentan-1-one (α-PVT), and their metabolites were determined in users' urine by liquid chromatography-tandem mass spectrometry using newly synthesized authentic standards. The identified metabolites indicated that metabolic pathways of three α-PVP analogues include the reduction of the carbonyl group to the corresponding alcohols and the oxidation of the pyrrolidine ring to the corresponding pyrrolidone, and 4MeO-α-PVP and α-PVT have additional metabolic pathways of the O-demethylation and the oxidation of thienyl group respectively. The quantitative analyses of the urinary metabolites suggested that the main metabolic pathways of these α-pyrrolidinophenones (PPs) derivatives could vary largely depending on the aromatic rings or substituent groups on the aromatic ring of PPs.

著者

掛橋 秀直 鎌田 寛恵 石川 亜香里 浅井 龍太郎 新田 篤志 和田 美暁 中野 史保子 松田 駿太朗 佐々木 啓子 志摩 典明 鎌田 徹 西岡 裕 三木 昭宏 片木 宗弘

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.24, no.1, pp.73-78, 2019 (Released:2019-01-31)

参考文献数

6

被引用文献数

2

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N-tert-Butoxycarbonyl-methamphetamine (t-BOCMA), a tert-butoxycarbonyl (t-BOC) derivative of methamphetamine (MA), which has recently been reported in several countries, was seized for the first time in Japan in 2017. It deprotected easily in an acidic condition to result in an illicit MA, and recently became a newly designated drug of the Pharmaceutical and Medical Device Act. For drug enforcement, the information of its properties was, therefore, strongly demanded. In this study, we synthesized the t-BOCMA standard, acquired various analytical data, and demonstrated its conversion to MA in high yield in the relatively moderate acidic condition (5% HCl methanol solution, 50℃). Also, the stability of t-BOCMA in simulated gastric juice (0.08 M HCl, 37℃) was explored by using GC/MS. As the result, 19% of t-BOCMA remained even after 120 min incubation, and the T1/2 was calculated to be 50 min. These suggest that the orally ingested t-BOCMA would be absorbed into blood in some degree without conversion to MA.