著者

坂本 美穂 蓑輪 佳子 岸本 清子 中嶋 順一 鈴木 仁 守安 貴子 深谷 晴彦 斉藤 貢一

出版者

公益社団法人 日本食品衛生学会

雑誌

食品衛生学雑誌 (ISSN:00156426)

巻号頁・発行日

vol.60, no.4, pp.96-107, 2019-08-25 (Released:2019-08-30)

参考文献数

36

被引用文献数

2

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LC/Tribrid Orbitrapを用いて強壮系健康食品中のphosphodiesterase-5 (PDE-5)阻害薬および構造類似体を迅速かつ確実に同定できる分析法を開発した.液体クロマトグラフの移動相に5 mmol/Lギ酸アンモニウム含有0.1%ギ酸溶液(pH 3)および0.1%ギ酸含有アセトニトリル溶液を使用し,C18カラムでPDE-5阻害薬および構造類似体を分離した後,higher-energy collisional dissociationおよびcollision-induced dissociationの2種類の解離法を用いて複数のMS/MSおよびMS3スペクトルを同時に取得した.本分析法を市販強壮系健康食品および個人輸入医薬品105検体に適用したところ,いずれの検体からもPDE-5阻害薬および構造類似体を検出することができた.さらに,検体から検出された3種類のPDE-5阻害薬の構造類似体と15種類のPDE-5阻害薬および構造類似体の不純物について,本分析法を用いて構造を推定した.本法は強壮系健康食品中に含まれるPDE-5阻害薬および構造類似体の迅速かつ確実な同定および構造推定に有用な方法である.

著者

守安 貴子 重岡 捨身 岸本 清子 石川 ふさ子 中嶋 順一 上村 尚 安田 一郎

出版者

公益社団法人日本薬学会

雑誌

藥學雜誌 (ISSN:00316903)

巻号頁・発行日

vol.121, no.10, pp.765-769, 2001-10-01

被引用文献数

13 35

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A substantially available identification system for Sildenafil in health foods was established using 3 different analytical mathods; i.e.TLC, preparative TLC/MS and HPLC/photo-diode array. Sildenafil in health foods was extracted with ethyl acetate under alkaline conditions as sample solutions for TLC and preparative TLC, and also extracted with 50% methanol and then diluted with solution of HPLC mobile phase for HPLC. The sample solution for TLC was applied to Silica gel 60 F_<254> plates with chloroform/methanol/28% ammonia(90:1:5, under layer)as mobile phase. Spots were located under UV radiation at 254 nm and 366 nm, and spraying dragendorff reagent. The conditions for preparative TLC were the same as these of TLC method, samples abtained from preparative TLC were determined by MS with APCI interface, under both positive and negative modes. The HPLC analysis was carried out on a column of Cosmosil 5C18-AR(4.6mm×150mm, 5μm)with 0.05 mol/l phosphate buffer pH 3.0/acetonitrile(73:27)as mobile phase and the eluate was monitored by a photo-diode array detector. The quantitative analysis was available, when the peak of this sample on HPLC was detected at 290nm. When this system was applied to commercial health foods, Sildenafil was identified and their contents were 25 mg-45 mg/tablet or bottle. These contents nearly correspond to that in Viagra, 25 mg, 50 mg/tablet. Therefore, there is a fear of side effects for Sildenafil, when it is taken as health foods.