著者

辻川 健治 岡田 侑己 瀬川 尋貴 山室 匡史 桑山 健次 金森 達之 岩田 祐子 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.103-113, 2021 (Released:2021-01-31)

参考文献数

13

被引用文献数

1

---

So-called “Ecstasy tablets” are tablets which are expected to contain 3,4-methylenedioxymethamphetamine (MDMA). However, they often contain different drugs such as methamphetamine (MA) and 4-bromo-2,5-dimethoxyphenethylamine (2C-B). A combination of Simon's reagent and Marquis reagent has been used as a field test for Ecstasy tablets in Japan. We examined the test performance for Ecstasy tablets. Mixtures of MDMA hydrochloride and lactose (1 or 5 mg), mixtures of MDMA hydrochloride and cellulose (1 mg) as well as pulverized Ecstasy tablets (1 mg) [main drugs: MDMA (n=39, 8.4 to 79.9% as MDMA hydrochloride), MA (n=9, 0.1 to 59.0% as MA hydrochloride), and 2C-B (n=6, 4.5 to 13.0% as 2C-B hydrochloride)] were placed on a white spot plate; then, the reagents were dropped. The color change was recorded by a digital camera. When 1 mg of the mixture of MDMA hydrochloride and the diluent was used, the lowest MDMA hydrochloride concentration giving positive was 25%, except when the combination of Simon's reagent and the mixture of MDMA hydrochloride and cellulose (1%) was used. When increasing the sample amount to 5 mg, enhancement of coloration for Marquis reagent was weaker than that for Simon's reagent because of the low sample solubility. All MDMA tablets was positive to Simon's reagent; however, 5 MDMA tablets, whose MDMA concentration was low (≤16.5% as MDMA hydrochloride), was negative for the Marquis reagent. Only 1 MA tablet (59% as MA hydrochloride) was positive for both tests. All 2C-B tablets were judged as negative for the Marquis reagent because of faint color change and influence of tablet color. We concluded that a combination of both reagents i) had acceptable sensitivity for MDMA tablets but may give some false negative results and ii) had insufficient sensitivity for MA tablets and 2C-B tablets. This study will provide useful information about the field test for Ecstasy tablets.

著者

山室 匡史 岡田 侑己 瀬川 尋貴 桑山 健次 辻川 健治 金森 達之 岩田 祐子

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.27, no.1, pp.73-83, 2022 (Released:2022-01-31)

参考文献数

11

被引用文献数

1

---

In Japan, possession of germinable cannabis seeds for cultivation purposes is subject to prosecution. Cannabis seeds are marketed after being treated to prevent germination (heated or crushed). Currently, forensic examination of cannabis seeds is conducted by cultivating the seeds after germination tests for several weeks and then performing morphological observation and chemical analysis on the true leaves. In this study, we attempted to construct a rapid and simple method for the identification of cannabis seeds by combining the color reaction using 2,3,5-Triphenyl-2H-tetrazolium Chloride (TTC), a reagent that discriminates between living and dead cells, and DNA testing using a commercially available simple kit. The color reaction using TTC can determine the viability of peeled embryos within 20 min at 45 ℃ as previously reported. This method is effective for quickly determining whether a seed has been heat-treated or not. However, in the color reaction, a commercial health food seed that claimed to be unheated showed some coloration. This sample had been crushed to prevent germination and was easily identified as non-germinable by morphological examination. After the color reaction, the embryos could be directly used for DNA extraction without washing, and the DNA testing could be carried out in about 2 hours by following the instruction manual of the kit. By following the above procedure, it was possible to identify in one day whether a seed was a germinable cannabis or not, without the need to cultivate the plant. This method is expected to make a significant contribution to improving the efficiency of cannabis seed analysis.

著者

岩田 祐子 桑山 健次 辻川 健治 金森 達之 井上 博之

出版者

公益社団法人 日本分析化学会

雑誌

分析化学 (ISSN:05251931)

巻号頁・発行日

vol.63, no.3, pp.221-231, 2014-03-05 (Released:2014-03-31)

参考文献数

27

被引用文献数

1 3

---

我が国で最も乱用されているmethamphetamineの塩酸塩について,押収されるまでの薬物の起源と履歴(原料,合成ルート,製造方法等)が反映されている薬物プロファイルを明らかにする薬物プロファイリングのこれまでの研究成果を報告する.アルカリ性下で有機溶媒を用いて微量成分を抽出しガスクロマトグラフィーを行う微量成分分析では,微量成分をよく検出・分離する条件を決定し,複数の内部標準物質を添加することにより,保持時間の補正精度を高めた.また,キャピラリー電気泳動法によるキラル分析では,覚醒剤や覚醒剤原料等のアンフェタミン型興奮剤9種を良好に分析する方法を確立し,methamphetamineに微量に含まれる原料ephedrine等もキラル分離して検出することが可能となった.さらに,methamphetamineの安定同位体比質量分析において,資料の関連性の評価基準を設定し,結晶ごとの測定の有効性を示した.各分析により,より詳細なプロファイルが得られ,異同識別や起源と履歴の推定に,より多くの情報が得られるようになっている.

著者

金森 達之 桑山 健次 辻川 健治 宮口 一 岩田 祐子 井上 博之 岸 徹

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.12, no.2, pp.237-245, 2007 (Released:2007-10-06)

参考文献数

7

被引用文献数

3 5

---

A urine sample obtained from a phenothiazine user was examined to identify metabolites which caused false-positive result on a screening test for methamphetamine in urine based on the Simon's color test. The urine sample was processed by liquid-liquid extraction under mild alkaline condition, and the extract was analyzed by TLC using Simon's reagent as a visualization reagent. Two blue or violet spots were appeared on the TLC plate by this reagent, and were identified as norchlorpromazine sulfoxide and norpromethazine sulfoxide by mass spectrometry after purification of the spots. Both of these two compounds possess an aliphatic secondary amine moiety, and are known as the metabolites of chlorpromazine and promethazine. These metabolites in the above urine sample were also confirmed by HPLC and LC/MS analysis. A control urine sample spiked with these metabolites gave positive result on the above screening test, indicating that these metabolites were the substances which caused false-positive on the test.

著者

岩田 祐子 桑山 健次 辻川 健治 金森 達之 井上 博之

出版者

公益社団法人 日本分析化学会

雑誌

分析化学 (ISSN:05251931)

巻号頁・発行日

vol.63, no.3, pp.221-231, 2014

被引用文献数

3

---

我が国で最も乱用されているmethamphetamineの塩酸塩について,押収されるまでの薬物の起源と履歴(原料,合成ルート,製造方法等)が反映されている薬物プロファイルを明らかにする薬物プロファイリングのこれまでの研究成果を報告する.アルカリ性下で有機溶媒を用いて微量成分を抽出しガスクロマトグラフィーを行う微量成分分析では,微量成分をよく検出・分離する条件を決定し,複数の内部標準物質を添加することにより,保持時間の補正精度を高めた.また,キャピラリー電気泳動法によるキラル分析では,覚醒剤や覚醒剤原料等のアンフェタミン型興奮剤9種を良好に分析する方法を確立し,methamphetamineに微量に含まれる原料ephedrine等もキラル分離して検出することが可能となった.さらに,methamphetamineの安定同位体比質量分析において,資料の関連性の評価基準を設定し,結晶ごとの測定の有効性を示した.各分析により,より詳細なプロファイルが得られ,異同識別や起源と履歴の推定に,より多くの情報が得られるようになっている.

著者

桑山 健次 辻川 健治 宮口 一 金森 達之 岩田 祐子 井上 博之 岸 徹 角田 紀子

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.10, no.2, pp.127-133, 2005 (Released:2007-07-03)

参考文献数

12

被引用文献数

1 1

---

The effects of the various preparation procedures of the Dragendorff reagent on sensitivity for thin layer chromatography (TLC) were examined. The sensitivity to various compounds was different depending on the preparation procedures of the Dragendorff reagent.   The reagent with the highest sensitivity to most of the compounds tested was the one prepared with bismuth subnitrate and concentrated hydrochloric acid. However, color spots were disappeared relatively in a short time after the reagent was sprayed on the compounds. The reagent with the second highest sensitivity was the one prepared with precipitation of Bi(OH)3 from bismuth subnitrate, although the procedure was complicated and time-consuming.   Consequently, to simplify the preparation procedure of the reagent, we modified it to the procedure without precipitation of Bi(OH)3 from bismuth subnitrate. The reagent was also prepared from commercially-manufactured Bi(OH)3 or BiI3. The modified Dragendorff reagents showed almost the same sensitivity to most of the compounds tested as the one prepared with precipitation of Bi(OH)3 from bismuth subnitrate, and would be useful for practical TLC analysis.

著者

岡田 侑己 瀬川 尋貴 山室 匡史 桑山 健次 辻川 健治 金森 達之 岩田 祐子

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.28, no.1, pp.51-58, 2023 (Released:2023-01-31)

参考文献数

9

被引用文献数

1

---

We examined the decomposition behavior of 1-acyl-substituted derivatives of d-lysergic acid diethylamide (LSD), such as 1-cyclopropanecarbonyl LSD (1cP-LSD), 1-acetyl LSD (ALD-52), and 1-propionyl LSD (1P-LSD) through gas chromatography/mass spectrometry (GC/MS). It was reported previously that in methanol, 1cP-LSD completely decomposed into LSD during GC/MS. We found that in methanol, 1cP-LSD remained undecomposed during GC/MS, and the extent of decomposition varied based on the analyses performed in this study. As a result of a detailed examination, we deduced that the decomposition occurs at the inlet, regardless of the inlet temperature or the type of the inlet liner. We observed that the peak areas of 1cP-LSD decreased with the deterioration of the inlet liner, and this was considered to be a cause for the variation between different analyses. While the acetonitrile solution of 1cP-LSD provided relatively robust results, the other examined solvents showed a significant decomposition of 1cP-LSD and/or a sequent decrease in the peak area of 1cP-LSD with time after the replacement of the inlet liner. ALD-52 or 1P-LSD in acetonitrile were stable during GC/MS, however, they were unstable when methanol was used as a solvent, similar to 1cP-LSD. This suggested that a similar decomposition and/or a sequent decrease in the peaks of ALD-52 and 1P-LSD during GC/MS can be expected.

著者

桑山 健次

出版者

公益社団法人 日本薬学会

雑誌

YAKUGAKU ZASSHI (ISSN:00316903)

巻号頁・発行日

vol.139, no.8, pp.1063-1070, 2019-08-01 (Released:2019-08-01)

参考文献数

39

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The abuse of drugs has become a serious social problem worldwide. Amphetamine-type stimulants such as methamphetamine are recreationally abused and can cause toxic effects in the body. Unfortunately, death from drug poisoning can occur due to careless intake. In postmortem examinations, the distribution of drugs in an entire organ gives valuable information for evaluating their toxicity. We developed methods to measure the distribution of drugs in organs using LC/MS and matrix-assisted laser desorption/ionization-imaging mass spectrometry (MALDI-IMS). The complementary use of the two methods provides more detailed information on the distribution and concentration of drugs in organs because the accurate quantification in LC/MS and small spatial resolution in MALDI-IMS are combined. On the other hand, it is important to elucidate the drug intake history of suspects and victims in drug-facilitated crimes (DFCs). Hair and nail samples are often used to confirm chronic drug intake because ingested drugs can stably remain in these specimens over several months. However, it is impossible to determine the day of drug ingestion in conventional segmental analysis of bulk samples. Therefore, we developed methods to cut hair strands at 0.4-mm intervals and nails at 0.2-mm intervals, which correspond to their respective growth rates over 1-2 d, to analyze the drugs in each segment efficiently using LC/MS. The microsegmental hair analysis method is applied to estimate the day of drug ingestion in DFC investigations. These methods could be applied to measure the distribution of compounds in various solid samples.

著者

山室 匡史 岡田 侑己 瀬川 尋貴 桑山 健次 辻川 健治 金森 達之 岩田 祐子

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.837, (Released:2022-06-16)

参考文献数

10

---

In Japan, forensic examination of cannabis seeds requires proof of “being cannabis” and “being germinable”, and is currently conducted by continuing cultivation of the seeds for several weeks after germination tests and performing morphological observations and chemical analysis on the true leaves. We have previously constructed a rapid and simple method for identification of cannabis seeds by combining the color reaction with DNA testing. In this study, the effectiveness of the cannabis seed identification methods by combining the color reaction, germination test, and DNA testing that does not involve a cultivation process was verified on seized cannabis seeds. As previously reported, the combination of the color reaction using 2,3,5-Triphenyl-2H-tetrazolium Chloride and DNA testing using a commercial kit proved that the seized materials were germinable cannabis seeds within one day. Furthermore, the germination test, in which the young roots and cotyledons were visually checked one week after sowing, was able to more directly confirm germination ability. In addition, DNA testing was possible for the young roots after germination, indicating that they were cannabis. This study shows that the methods of cannabis seed identification, which does not involve a cultivation process, are effective even for seized materials whose storage conditions are unknown.

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

金森 達之 岩田 祐子 瀬川 尋貴 山室 匡史 桑山 健次 辻川 健治 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.24, no.2, pp.123-133, 2019 (Released:2019-07-31)

参考文献数

13

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The isomers of fluoro-butyrylfentanyl, fluoro-isobutyrylfentanyl, and fluoro-methoxyacetylfentanyl, in which the position of fluorine on the N-phenyl ring varies, were synthesized, characterized, and differentiated by infrared (IR) spectroscopy, liquid chromatography/mass spectrometry (LC/MS), and gas chromatography/mass spectrometry (GC/MS). The isomers could be clearly differentiated by their IR spectra. In the LC/MS chromatograms, the separation of the fluoro-butyrylfentanyl and fluoro-isobutyrylfentanyl isomers was insufficient. However, in the GC/MS extracted ion chromatograms, all compounds were completely separated. The LC/MS and GC/MS mass spectra of the isomers were similar, demonstrating that it is difficult to distinguish the positional isomers of fluorinated fentanyl analogs by their mass spectra.

著者

金森 達之 桑山 健次 辻川 健治 宮口 一 岩田 祐子 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.91-101, 2014 (Released:2014-07-30)

参考文献数

12

被引用文献数

1 1

---

The in vivo metabolism of 2,5-dimethoxy-4-ethylthiophenethylamine (2C-T-2) and 2,5-dimethoxy-4-isopropylthiophenethylamine (2C-T-4), new psychoactive drugs, were studied using rats. 2C-T-2 hydrochloride and 2C-T-4 hydrochloride were administered separately to male Sprague-Dawley rats via the oral route (10 mg/kg), and the urinary extracts were analyzed by liquid chromatography/mass spectrometry. Fourteen and ten metabolites for 2C-T-2 and 2C-T-4 were detected in the urinary extracts, respectively. Our results suggested that sulfoxidation, sulfone formation, S-dealkylation followed by S-methylation, N-acetylation and deamination followed by oxidation were the major metabolic pathways of 2C-T-2 and 2C-T-4 in rat.

著者

金森 達之 岩田 祐子 辻川 健治 桑山 健次 山室 匡史 瀬川 尋貴 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.21, no.2, pp.139-147, 2016 (Released:2016-07-23)

参考文献数

16

被引用文献数

1 3

---

Simultaneous analytical methods for 18 compounds of fentanyl and its analogues by thin-layer chromatography (TLC), gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS) were developed. In TLC, fentanyl analogues were well separated by using toluene-acetone-28% aq. ammonia (20:10:0.3, by vol.) as a developing solvent. In GC/MS, fentanyl analogues, except for fentanyl and acetyl-α-methylfentanyl, could be separated on the extracted ion chromatograms (EIC) of the characteristic fragment ions of each compound. In LC/MS, fentanyl analogues could be separated on the EICs of the protonated molecule of each compound. All of the fentanyl analogues tested were identified correctly by using the combination of TLC, GC/MS and LC/MS.

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

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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.