著者

角田 紀子

出版者

一般社団法人 日本質量分析学会

雑誌

Journal of the Mass Spectrometry Society of Japan (ISSN:13408097)

巻号頁・発行日

vol.53, no.3, pp.157-163, 2005 (Released:2006-04-05)

参考文献数

38

被引用文献数

1 3

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2004 was the 10th anniversary of the Matsumoto sarin incident, and 2005 is the 10th anniversary of the Tokyo Subway Attack. National Research Institute of Police Science has been engaged in forensic examinations into these incidents. Chemical analyses of the victim's blood, water, soil, and wipe samples were performed by organic solvent extraction, followed by gas chromatography-mass spectrometry with or without tert-butyldimethylsilylation. As a result, sarin and its hydrolysis products (isopropylmethyl phosphonate and methylphosphonate), derived from sarin were positively identified by their mass spectra and retention indices. Furthermore, from the chemical analysis of evidence samples taken from the scene of manufacturing plant, precusors, and byproducts corresponding to synthetic routs of sarin has been identified. This paper presents characteristics of nerve agents, sample preparation of sarin, optimization of GC-MS, and case reports from a standpoint of effectiveness of GC-MS.

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

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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

太田 彦人 瀬戸 康雄 角田 紀子

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.39, no.2, pp.155-160, 1993

被引用文献数

2

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The determination and confirmation of trans-10-hydroxydecenoic acid (10-HDA) in royal jelly (RJ) were developed by capillary gas chromatography (GC) and GC-chemical ionization mass spectrometry (CI-MS) equipped with an ion trap detector (ITD) as a mass spectrometer. It was found that 10-HDA extracted with dichloromethane at pH 2.5 was converted into trimethylsilyl (TMS) derivative in a constant yield by the reaction with N, O-bis (trimethylsilyl) acetamide at room temperature for 15 min. The recovery of 10-HDA (50 μg) was 99.5%. The TMS derivatives of raw RJ tested showed a satisfactory result of separation and sensitivity by GC using a DB-1 capillary column with a flame ionization detector. The linear dynamic detection range was approximately from 50 ng to 500 μg (16.7-167000 ppm) determined using n-eicosane as an internal standard. The minimum detectable amount of 10-HDA was found to be 50 ng (16.7 ppm) at the split ratio of 40 : 1 of the split injection. The amount of 10-HDA in the raw RJ sample was 2.28±0.04% determined by the GC method and 2.25±0.01% by the HPLC method as described previously, respectively. The TMS derivatives of 10-HDA and its related compounds in the raw RJ were confirmed by ITD-GC. The diagnostic ions of TMS-HDA were presented at m/z 331 (M+1), 315 (M-Me), and 241 (M-OTMS) in isobutane CI mode. The present GC method is an easier and more convenient method for the analysis of 10-HDA in RJ and is applicable for the determination and confirmation of 10-HDA in forensic and food samples.

著者

斯波 久二雄 角田 紀子 金子 秀雄 中塚 巌 吉武 彬 山田 宏彦 宮本 純之

出版者

日本農薬学会

雑誌

日本農薬学会誌 (ISSN:03851559)

巻号頁・発行日

vol.13, no.4, pp.557-569, 1988-11-20

被引用文献数

2

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新規ピレスロイド系殺虫剤S-4068SF [Etoc^[○!R], (S)-2-methyl-4-oxo-3-(2-propynyl)cyclopent-2-enyl (1R)-trans/cis-chrysanthemate, (trans/cis=8/2)]の代謝運命を明らかとするため, (4S, 1R)-trans-または(4S, 1R)-cis-S-4068のアルコール側^<14>C標識体を2 mg/kgの割合で, 雌雄ラットに1回経口または皮下投与した.放射能は, 投与後7日間で完全に糞尿中に排泄された.血液および組織中^<14>C濃度は, 経口投与後3時間以内に最大値を示したのち, 生物学的半減期は, 投与後3時間から12時間まで3時間ないし5時間, 12時間から48時間まで7時間ないし35時間で減少した.投与7日後の組織残留量は, 全般的に低値を示した.排泄物中, 20種類の代謝物を同定し, 代謝経路を以下のように推定した.1) 酸側イソブテニルのメチル基およびアルコール側プロピニル基の1位および2位の酸化, 2) エステル結合の開裂, 3) 以上の結果生成した化合物のグルクロン酸または硫酸による抱合.両異性体の代謝運命に, 雌雄および投与経路によらず顕著な差異を認めなかった.