title: Determination and purification of sesamin and sesamolin in sesame seed oil unsaponified matter using reversed-phase liquid chromatography coupled with photodiode array and tandem mass spectrometry and high-speed countercurrent chromatography.
abstract: In Asian countries, sesame seed oil unsaponified matter is used as a natural food additive due to its associated antioxidant effects. We determined and purified the primary lignans sesamin and sesamolin in sesame seed oil unsaponified matter using reversed-phase liquid chromatography coupled with photodiode array and tandem mass spectrometry and high-speed countercurrent chromatography. Calibration curves showed good correlation coefficients (r2> 0.999, range 0.08 and/or 0.15 to 5 μg/mL) with a limit of detection (at 290 nm) of 0.02 μg/mL for sesamin and 0.04 μg/mL for sesamolin. Sesame seed oil unsaponified matter contained 2.82% sesamin and 2.54% sesamolin, respectively. Direct qualitative analysis of sesamin and sesamolin was achieved using quadrupole mass spectrometry with positive-mode electrospray ionization. Pure (>99%) sesamin and sesamolin standards were obtained using high-speed countercurrent chromatographic purification (hexane/ethyl acetate/methanol/water; 7:3:7:3). An effective method for determining and purifying sesamin and sesamolin from sesame seed oil unsaponified matter was developed by combining these separation techniques for standardized food additives.
authors: Laboratory of Clinical & Analytical Chemistry, College of Pharmaceutical Sciences, Ritsumeikan University, Kusatsu, Shiga, Japan.
authors: Miki
authors: M
authors: Takahashi
authors: National Institute of Health Sciences, Setagaya-ku, Tokyo, Japan.
authors: Yuzo
authors: Y
authors: Nishizaki
authors: National Institute of Health Sciences, Setagaya-ku, Tokyo, Japan.
authors: Naoki
authors: N
authors: Sugimoto
authors: Nagaoka Perfumery Co., Ltd, Chuo-ku, Osaka, Japan.
authors: Hiroaki
authors: H
authors: Takeuchi
authors: Nagaoka Perfumery Co., Ltd, Chuo-ku, Osaka, Japan.
authors: Kazuya
authors: K
authors: Nakagawa
authors: National Institute of Health Sciences, Setagaya-ku, Tokyo, Japan.
authors: Hiroshi
authors: H
authors: Akiyama
authors: National Institute of Health Sciences, Setagaya-ku, Tokyo, Japan.
authors: Kyoko
authors: K
authors: Sato
authors: Laboratory of Clinical & Analytical Chemistry, College of Pharmaceutical Sciences, Ritsumeikan University, Kusatsu, Shiga, Japan. kinoue@fc.ritsumei.ac.jp.
authors: Koichi
authors: K
authors: Inoue
mesh_terms: D056148:Chromatography, Reverse-Phase; D003377:Countercurrent Distribution; D004149:Dioxoles / Q000302:isolation & purification*; D017705:Lignans / Q000302:isolation & purification*; D012715:Sesame Oil / Q000032:analysis*; D031685:Sesamum / Q000737:chemistry; D053719:Tandem Mass Spectrometry
chemical_list: D004149:Dioxoles; D017705:Lignans; C054124:sesamolin; D012715:Sesame Oil; C054125:sesamin
keywords: Food additives; High-speed countercurrent chromatography; Sesamin; Sesamol; Sesamolin