健康食品中西地那非(伟哥)的HPLC测定
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健康食品中西地那非(伟哥)的
HPLC测定
Identification System for Sildenafil in Health Foods
(摘引自YAKUGAKU ZASSHI 121(10) 765―769 (2001) 765)
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
東京都立衛生研究所理化学部
Takako MORIYASU, Sutemi SHIGEOKA, Kiyoko KISHIMOTO, Fusako ISHIKAWA, Jyunichi NAKAJIMA, Hisashi KAMIMURA, and Ichiro YASUDA
The Tokyo Metropolitan Research Laboratory of Public Health, 3241,
Hyakunin-cho, Shinjuku-ku, Tokyo 1690073, Japan
(Received May 1, 2001; Accepted August 1, 2001)
A substantially available identification system for Sildenafil in health foods was established using 3 diŠerent analytical methods; 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 F254 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 dragendorŠ reagent. The
conditions for preparative TLC were the same as these of TLC method, and 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(4.6 mm×150
mm, 5 mm) 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 290 nm.When this system was applied to commercial health foods, Sildenafil was identiˆed
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 efects for Sildenafil, when it is taken as health foods.
Key words―Sildenafil; health foods; preparative TLC/MS; TLC; HPLC/photo-diode array
HPLC Chromatograms of Sildenafil in Health Foods
1: sildenafil standard, 2: sample 1, 3: sample 2, 4: sample 3.