2 0 0 0 OA ヘッドスペース-ガスクロマトグラフィー―窒素リン検出による飲料中シアンの分析
- 著者
- 大塚 麻衣 山口 晃巨 数井 優子 西田 響 大森 毅 宮口 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.28, no.2, pp.169-176, 2023 (Released:2023-07-31)
- 参考文献数
- 14
Cyanide is a gaseous poison which is liberated from cyanide compounds such as potassium cyanide. In spite of high toxicity, cyanide compounds are easily accessible for industrial use, and some contamination cases of cyanide into beverages have occurred. For analysis of cyanide, various analytical methods such as colorimetric methods have been reported. Among those, headspace-gas chromatography-nitrogen phosphorus detection (HS-GC-NPD) is known for its easy pretreatment method and high quantitation ability. The application of HS-GC-NPD analysis to cyanide in blood specimens have been reported by many groups. However, comparison results of some experimental manipulations, such as addition of acid, syringes used for introduction of samples to the GC, and amount of sample introduced into the GC are not clear. In addition, there is no detailed description about application to beverage samples. In this work, we have investigated some experimental manipulation of manual HS-GC-NPD and applied the optimized method to beverage samples. After the optimization, the addition of acid with micropipette in open system and introduction of 100 μL of headspace gas into GC with gastight syringe are recommended. For beverage samples, although variations were larger than standard samples, those variations could be compensated by use of acetonitrile as an internal standard.
2 0 0 0 OA フェノチアジン系薬物摂取者尿中のシモン反応陽性代謝物の同定
- 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.
1 0 0 0 OA 薄層クロマトグラフィーにおけるドラーゲンドルフ試液調製法の違いによる検出感度への影響
- 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
- 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.