Ergot alkaloids, separation

Ergot alkaloids Separation with straight phase ion-pair HPLC (Tables 9.9, 9.10) ifiondapak CN 300x3.9 Hexane-CHCl -ACN-di-(2-ethyl -hexyl)phospnoric acid in various ratios 61... 

Isolation of Ergot Alkaloids. In the papers already quoted (refs. 6 to 19) the processes used for the isolation of the total alkaloids and the separation of the component bases are given to those may be added references to methods by other authors. There are also numerous patented processes, some of which are quoted in the following special sections. 

Frach, K., and Blaschke, G. (1998). Separation of ergot alkaloids and their epimers and determination in sclerotia by capillary electrophoresis. /. Chromatogr. A 808, 247—252. 

An extremely important aspect in pharmaceutical research is the determination of drug optical purity. The most frequently applied technique for chiral separations in CZE remains the so-called dynamic mode where resolution of enantiomers is carried out by adding a chiral selector directly into the BGE for in situ formation of diastereomeric derivatives. Various additives, such as cyclodextrins (CD), chiral crown ethers, proteins, antibiotics, bile salts, chiral micelles, and ergot alkaloids, are reported as chiral selectors in the literature, but CDs are by far the selectors most widely used in chiral CE. 

High-performance liquid chromatography on silica is recommended470 for the separation of some, but not all, mixtures of ergot alkaloids an improved procedure, which is claimed to be satisfactory for the separation and determination of mixtures of cyclol ergot alkaloids obtained from fermentation media, involves the use of silica gel modified with alkylamines as the stationary phase, with gradient elution by diethyl ether-ethanol mixtures.476... 

The separation of the naturally occurring ergot alkaloids derived from lysergic acid in... 

The first reversed-phase separation of ergot alkaloids was reported by Jane and Wheals in connection with the analysis of LSD. Pellicular beads with chemically bonded octadecyl groups were used in combination with methanol - 0.1% aqueous ammonium carbonate (3 2) as mobile phase However, the mobile phase proposed by Vivilecchia et al.6 for the separation of the dihydro-ergotoxine alkaloids on octadecyl columns (acetonitrile - aqueous ammonium carbonate) has been... 

CAPACITY FACTORS (k ) AND SEPARATION FACTORS FOR ERGOT ALKALOIDS ON REVERSED-PHASE PACKINGS25,34... 

Dolinar found that the packing with chemically bonded octyl groups was the most suitable stationary phase for the separation of ergot alkaloids with a wide range of polarities (Fig.9.1). The separations obtained on an octadecyl column were similar (Fig.9.2). On a dimethylsilyl column (RP2) and a spherical octadecyl column (Spherisorb 0DS), the less polar alkaloids were not as well separated as on the above-mentioned columns however, the more polar alkaloids were... 

CAPACITY FACTORS AND SEPARATION FACTORS (a) FOR SOHE ERGOT ALKALOIDS ON A REVERSED PHASE C0LUMN39... 

Jane separated a wide range of drugs of abuse on microparticulate silica gel with polar mobile phases containing ammonium nitrate solutions. LSD could be analyzed with methanol -0.2 M ammonium nitrate solution (3 2)(Fig.9.6). The system has been successfully applied to the analysis of ljd13 15 16 28 45 46, but for the analysis of ergot alkaloids the above mentioned reversed-phase system gave better results3 (Table 9.5). 

Quercia et al. used a microparticulate aluminium oxide column to separate the dihydroderivatives of some ergot alkaloids and pentane - methanol (98 2) or (97 3) as mobile phase. 

The present invention relates to the manufacture, separation and preparation of ergot-alkaloids in state of high purity, by subjecting mixtures of the very sensitive ergot-alkaloids to chromatographic adsorption analysis. 

Ergotamin [a]20°/D = -155° and Ergotaminin [a]20°/D =-i-381°), it is easy to control the separation of the two alkaloids by means of the polarimetric method. It is also possible to control the separation of the alkaloids by irradiating their solutions with ultraviolet light, as it is known that in this light the ergot-alkaloids possess a violet to blue fluorescence. 

All the known processes heretofore used for the separation and preparation of pure ergot alkaloids are completely different from the process herein described, as indifferent adsorption media used in the process of Tswett have never been used for this purpose. The possibility of separating and of preparing the very sensitive ergot-alkaloids even from impure mixtures by the chromatographic process and without the use of any chemical reagents, represents a very valuable process and a great improvement of the art. 

One object of the present invention is, therefore, a process for the manufacture, separation and preparation of pure ergot-alkaloids, consisting in subjecting raw or pure mixtures of ergot alkaloids or impure ergot-alkaloids to the chromatographic adsorption process. 

Stoll, A. Process for the Manufacture, Separation and Preparation of Pure Crystallized Ergot-Alkaloids 1937 US 2,080,954... 

---