Simultaneous Analysis of Seven Benzodiazepines in Dietary Supplements as Adulterants Using High Performance Liquid Chromatography and its Application to an Identification System for Diazepam

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概要

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• A high performance liquid chromatography (HPLC) method for the simultaneous analysis of the seven benzo-diazepines (BZDs), oxazolam, nitrazepam, oxazepam, tofisopam, triazolam, clotiazepam and diazepam (DIA) is presented for application in the screening examination of dietary supplements as adulterants. Samples were analyzed after extraction with methanol. HPLC analysis was performed with on a column of Wakosil 5C18 (4.6×150mm, 5μm) with the mobile phase consisting of 1-heptanesulfonic acid sodium salt 5mM dissolved in water/acetonitrile 1000ml (13:7, v/v), adjusted with phosphoric acid to pH 2.4. The column eluent was monitored with a photodiode array detector, and the quantitative analysis of BZDs was performed at 225nm. The calibration curves of the seven BZDs showed good linearity and the correlation coefficients were better than 0.999 in all cases. When this procedure was applied to commercial supplements, an DIA-adulterated capsule-type supplement was detected. Finally, DIA was identified and determined using a combination of three different analytical methods: HPLC/photodiode array, thin-layer chromatography (TLC), and LC/MS. DIA was present at a concentration of 1.9 mg/capsule. The procedure described here can provide a broad analysis in a single run within 17 min and is available for the screening of seven BZDs in adulterated supplements with minimal sample preparation.

• 公益社団法人日本薬学会の論文
• 2005-06-01

著者

• OKA Hisao

  Aichi Prefectural Institute of Public Health

• GOTO Tomomi

  Aichi Prefectural Institute of Public Health

• Oka Hisao

  Dep. Of Toxicology Aichi Prefectural Inst. Of Public Health

• Goto Tomomi

  Department of Toxicology, Aichi Prefectural Institute of Public Health

• KANAMORI Hisayuki

  Hiroshima Prefectural Institute of Public Health and Environment

• Ohno Tsutomu

  Aichi Prefectural Institute Of Public Health

• MIKAMI Eiichi

  Aichi Prefectural Institute of Public Health

• Goto Tomomi

  岡山大学 医歯薬学総合研究科免疫医薬品化学

• Kanamori Hisayuki

  Hiroshima Prefectural Health Environment Center

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