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

---

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

山室 匡史 宮本 重彦 立入 直紀 石井 歩 松田 駿太朗 岩田 祐子 瀬川 尋貴 桑山 健次 辻川 健治 金森 達之 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.26, no.1, pp.29-48, 2021 (Released:2021-01-31)

参考文献数

31

被引用文献数

3 1

---

The forensic identification of cannabis is performed by a combination of chemical analysis and morphological examination. Recently, molecular biological analysis using cannabis DNA information has been noticed as a new approach. In this study, the cannabis DNA detection kit using a DNA chromatography chip was developed, and the demonstration evaluation in the forensic chemical laboratory was carried out. The DNA detection kit of a “four-line version” which had the function to distinguish fiber-type from drug-type cannabis showed as high accuracy (98.3%) as the current identification method on cannabis identification. However, there was a tendency to mistake a part of the drug-type samples as “fiber-type cannabis”. In the kit of a “three-line version” which was specialized for the cannabis DNA detection, the accuracy of 99.0% was confirmed on the cannabis identification. There were no false positives throughout all evaluations. In addition, some of the combustion residues that could not be identified as cannabis by the current identification method were classified to be “cannabis positive” by the DNA detection kit, indicating the effectiveness of a new approach. As a result of this study, it was shown that the quick and accurate cannabis DNA analysis could be carried out by the DNA detection kit even by analytical chemists who didn't have expertise in molecular biology.

著者

山室 匡史 宮本 重彦 立入 直紀 石井 歩 松田 駿太朗 岩田 祐子 瀬川 尋貴 桑山 健次 辻川 健治 金森 達之 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

pp.786, (Released:2020-09-14)

参考文献数

31

被引用文献数

1

---

The forensic identification of cannabis is performed by a combination of chemical analysis and morphological examination. Recently, molecular biological analysis using cannabis DNA information has been noticed as a new approach. In this study, the cannabis DNA detection kit using a DNA chromatography chip was developed, and the demonstration evaluation in the forensic chemical laboratory was carried out. The DNA detection kit of a “four-line version” which had the function to distinguish fiber-type from drug-type cannabis showed as high accuracy (98.3%) as the current identification method on cannabis identification. However, there was a tendency to mistake a part of the drug-type samples as “fiber-type cannabis”. In the kit of a “three-line version” which was specialized for the cannabis DNA detection, the accuracy of 99.0% was confirmed on the cannabis identification. There were no false positives throughout all evaluations. In addition, some of the combustion residues that could not be identified as cannabis by the current identification method were classified to be “cannabis positive” by the DNA detection kit, indicating the effectiveness of a new approach. As a result of this study, it was shown that the quick and accurate cannabis DNA analysis could be carried out by the DNA detection kit even by analytical chemists who didn't have expertise in molecular biology.

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

---

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

---

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

---

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.

著者

松田 駿太朗 片木 宗弘 西岡 裕 鎌田 寛恵 佐々木 啓子 志摩 典明 鎌田 徹 三木 昭宏 辰野 道昭 財津 桂 坪井 健人 土橋 均 鈴木 廣一

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.77-89, 2014 (Released:2014-07-30)

参考文献数

12

被引用文献数

12 19

---

Cathinone-type designer drugs are a newly-encountered drug family that has a β-ketophenethylamine skeleton. Recently, the abuse of these drugs has been increasingly common among young adults, and this has caused a serious social problem in many countries. Many of those drugs have become regulated by the Pharmaceutical Affairs Act, and some of them were later banned by the Narcotics and Psychotropics Control Act in Japan, depending on their structures. In this paper, a total of 98 standards of cathinone-type designer drugs were synthesized, and their EI-mass spectra were acquired by GC/MS, with and without trifluoroacetylation. For their free bases, a major fragment ion formed from the α-cleavage of the amine nitrogen was commonly observed. Also, a small fragment ion generated by the α-cleavage of the carbonyl group, followed by the elimination of CO was detectable. For the analogs having an N-alkyl chain longer than methyl group and/or the alkyl side-chain longer than methyl group, a characteristic ion formed from the α-cleavage of the amine nitrogen, followed by the elimination of the olefin moiety was observed. For the trifluoroacetyl derivatives, the intensity of fragment ion formed from the α-cleavage of carbonyl group significantly increased, while that of the fragment ion generated from the α-cleavage of nitrogen decreased, when compared with those of free bases. Also, the ion at m/z 110 was specifically observed for the cathinone analogs having a methylamino group. Those typical fragmentation patterns revealed by analyzing a series of analogs provide useful information for the characterization of cathinone-type designer drugs.