β-Naphtoquinone(BNQ)プレラベル化法による唾液中のメタンフェタミン及びその代謝物のHPLC分析
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概要
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A high-performance liquid chromatographic rapid analytical method with β-naphthoquinone (BNQ) prelabelling for the simultaneous determination of methamphetamine (MA) and its metabolite, amphetamine (AP), in saliva has been studied. Without pretreatment, the direct derivatization of amphetamines in saliva has been developed. As a result of study on the optimization of the derivatization, a reaction mixture of 100μl of saliva containing MA and AP, 200μl of 0.5% Na_2CO_3,200μl of aq. solution of 0.5% BNQ-sulfonate, 200μl of methoxyphenamine (1μg/ml) as an internal standard and 100μl of methanol, as a shift agent of interference peak was warmed at 40℃ for 20 min. The reaction solution was extracted with n-hexane-ether (1 : 1) and the solvent was evaporated under N_2. The residue dissolved in acetonitrile was analysed by high-performance liquid chromatography on a column of μBondasphere C_<18> with acetonitrilemethanol-0.01M H_2SO_4 (20 : 20 : 67) as a mobile phase (0.8ml/min) and electrochemical detection at -0V. Calibration curves were rectilinear for 50 to 10000ng/ml of MA and AP in saliva. By this method, 6 saliva samples of 4 male and 1 female human suspects who had taken i. v. dose of MA hydrochloride at 7.3,7.8,10.2,20.4,31 and 66.5h earlier were analysed to confirm the use of MA. Until at least 31h after use, MA and AP were detected at 0.1 to 24.8μg/ml. Comparing with urine and blood samples, the usefulness of the saliva sample was disccused.
- 公益社団法人日本薬学会の論文
- 1991-12-31
著者
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関根 均
Criminal Investigation Laboratory Saitama Pref. Police H.q.
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関根 均
埼玉県警・科搜研
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中原 雄二
国立衛生試験所
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中原 雄二
National Institute Of Health Sciences
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