Chromatography Saponins

The identities of the individual sugars were established by acid hydrolysis of a portion of the sample followed by paper chromatography and comparison with authentic samples. It was interesting to note that one of the sugars was the rarely encountered (S-D-allose that has only been found in a few saponins. Regrettably, only scant details were reported on the acquisition conditions used for the 1,1-ADEQUATE spectrum. 

Asafu-Adjaye, E. B. and Wong, S. K. (2003). Determination of ginsenosides (ginseng saponins) in dry root powder from Panax ginseng, Panax quinquefolius, and selected commercial products by liquid chromatography Interlaboratory study. /. AOAC Int. 86, 1112-1123. 

Cui, M., Song, F., Zhou, Y., Liu, Z., and Liu, S. (2000). Rapid identification of saponins in plant extracts by electrospray ionization multi-stage tandem mass spectrometry and liquid chromatography/tandem mass spectrometry. Rapid Commun. Mass Spectrom. 14, 1280-1286. 

Samukawa, K., Yamashita, H., Matsuda, H., and Kubo, M. (1995). Simultaneous analysis of saponins in ginseng radix by high performance liquid chromatography. Chem. Pharm. Bull 43, 137-141. 

Wang, C.-Z., Wu, J. A., McEntee, E., and Yuan, C.-S. (2006a). Saponins composiKon in American ginseng leaf and berry assayed by high-performance liquid chromatography. /. Agric. Food Chem. 54, 2261-2266. 

Zhang, H., and Cheng, Y. (2006). Solid-phase extraction and liquid chromatography-electrospray mass spectrometric analysis of saponins in Chinese patent medicine of formulated Salvia miltiorrhizae and Panax notoginseng. J. Pharm. Biomed. Anal. 40,429 32. 

When micelles are used, the CE technique becomes a micellar elec-trokinetic chromatography (MEKC) one. Natural surfactants, such as bile salts, digitonin and saponins, optically active synthetic surfactants, e.g., amino-acid derived ones, alkylglycoside-, tartaric acid- and steroidal glucoside-based surfactants, and high-molecular mass or polymerized surfactants, have been used as chiral selectors in In the lat-... 

Centrifugal partition chromatography (CPC) relies on centrifugal force rather than gravitation for the retention of the stationary phase and solvents can be pumped at higher speeds through the instruments. In addition, no need for droplets formation is required. This allows shorter separation times, without loss of resolution, and an infinite choice of solvents with the only requirement of forming two immiscible phases, stable with the time. Chloroform-based systems have been mostly used for the separation of saponins due to their favourable partition coefficient towards such solvents. [116, 119, 120]. 

In our laboratory, an on-flow LC-NMR-MS screening (Figure 5.1.1) was applied to both saponin fractions which were not separated into pure compounds by classical column chromatography and further to total asterosaponin fractions obtained by the micropreparative technique, matrix solid-phase dispersion (MSPD) extraction [45] (see Figure 5.1.2). The LC-NMR-MS hyphenation is set up in the widely used parallel configuration of NMR and mass spectrometer (Figure 5.1.3). Typically, absolute amounts of asterosaponin mixtures of about 500 xg - 1 mg are injected onto the column. 

Ireland, P.A., Dziedzic, S.Z., and Kearsley, M.W. 1986. Saponin content of soya and some commercial soya products by means of high-performance liquid chromatography of the sapogenins. 

T. Renukappa, G. Roos, I. Klaiber, B. Vogler, and W. Kraus, Application of high-performance liquid chromatography coupled to nuclear magnetic resonance spectrometry, mass spectrometry and bioassay for the determination of active saponins from Bacopa Monniera Wettst.,7. Chromatogr. A 847 (1999), 109-116. 

Gas chromatography-mass spectrometry parameters for anabolic steroid metabolites, " steroid alkaloids and saponins, and their MS data were published previously. 

Lau, A., Woo, S., and Koh, H.L. 2003. Analysis of saponins in raw and steamed Panax notoginseng using high-performance liquid chromatography with diode array detection. J. Chromatogr. A. 1011, 77-87. 

Yoshikawa et al. isolated the crude saponin from G. syLvestrs=as follows The dried leaves were extracted with 60% EtOH at 60°C for two weeks. The EtOH extract obtained after evaporation of the solvent in vacuo was passed through an Amberlite XAD-2 column and eluted with MeOH. The MeOH eluate was psssed through Toyopearl HW-40 column (MeOH) to give the crude saponin. The crude saponin was further fractionated by chromatography on Servachrome XAD-2 (elution with 40-70% MeOH). 

Imoto et al. by high performance liquid chromatography combined with atmospheric pressure ionisation mass spectrometry (API-MS). The crude saponin isolated from the leaves was chromatographed on octadecyl silica column and eluted with an aqueous methanol solution containing ammonium acetate. The fractions thus separated were directly introduced into an atmospheric pressure ionisation mass spectrometer connected with the liquid chromatograph by an interface consisting of a nebulizer and a vaporizer through a PTFE tube (Hitachi, Japan). The vaporized sample and solvent molecules at 300°C were introduced into the ion source of the atmospheric pressure ionisation system. 

Fora precise differentiation, chromatography must be performed in the saponin solvent system chloroform-glacial acetic acid-methanol-water (64 32 12 8). 

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