Determination of the content and purity of ergotamine preparations by means of high-pressure liquid chromatography

Bethke, H.; Delz, B.; Stich, K.

doi:10.1016/s0021-9673(00)81115-2

Cited by 40 publications

(6 citation statements)

References 6 publications

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“…The fact that ergot alkaloids possess different amine functions requires the use of buffered mobile phase systems and performed by either isocratic elution [6,8,14,[24][25][26][28][29][30] or in the gradient mode [1,[7][8][9]13,15,16,25] on C 18 and C 8 columns. In some applications acetonitrile-10 mM ammonium carbonate mixtures [1,9,13,24,25,28] were used but except Ref.…”

Section: Sample Preparation Chromatographic Separation and Detectionmentioning

confidence: 99%

“…In some applications acetonitrile-10 mM ammonium carbonate mixtures [1,9,13,24,25,28] were used but except Ref. [24] no indications are made with respect to long-term stability of the chromatographic support under the slightly alkaline conditions of the mobile phase.…”

Section: Sample Preparation Chromatographic Separation and Detectionmentioning

confidence: 99%

“…However, liquid chromatographic procedures, coupled to mass spectroscopic detection (MSD), provide some crucial advantages, in particular with concern to specificity. Indeed, high performance liquid chromatographic methods [1,[6][7][8][9]13,[15][16][17][24][25][26][27][28][29][30] prevail in analytical investigations of ergot alkaloids targeted either to get more precise insight into the metabolic pattern or to obtain thorough information of their concentrations in a biological environment, such as, e.g., serum or plasma, urine, tissue, etc. Among them three methods apply the selective "on-line" LC-MS hyphenation [13,15,17] allowing direct and unequivocal structural assignment of the compounds of interest even in those cases where co-elution of two or more species occurs provided ionization energy is not quantitatively consumed by the interfering ones.…”

Section: Introductionmentioning

confidence: 99%

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Determination of dihydroergocryptine in human plasma and urine samples using on-line sample extraction?column-switching reversed-phase liquid chromatography?mass spectrometry

Friedrich¹,

Appel²,

Rose³

et al. 2004

Journal of Chromatography B

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Section: Sample Preparation Chromatographic Separation and Detectionmentioning

confidence: 99%

Section: Sample Preparation Chromatographic Separation and Detectionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Determination of dihydroergocryptine in human plasma and urine samples using on-line sample extraction?column-switching reversed-phase liquid chromatography?mass spectrometry

Friedrich¹,

Appel²,

Rose³

et al. 2004

Journal of Chromatography B

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“…Flow rate: 1.0 ml/ rain. Detection wavelength: 320 nm (Bethke et al 1976). Samples: 5 ml atcalized medium supernatant was extracted threefold with 10 ml chloroform each time.…”

Section: Determination Of Ergot Alkaloids By Hplc Hplc Was Carried Outmentioning

confidence: 99%

Influence of inorganic phosphate and immobilization on Claviceps purpurea

Lohmeyer

Dierkes

Rehm

1990

Appl Microbiol Biotechnol

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The influence of inorganic phosphate and immobilization on cells of Claviceps purpurea strain 1029/N5 producing ergot peptides in shake culture was examined. Immobilization in Ca-alginate beads resulted in a marked reduction of some metabolic activities, i.e. the periods of alkaloid formation and cell growth were prolonged. High concentrations of inorganic phosphate (1 g/l KHzPO4) could reduce or stop alkaloid formation both by free and immobilized cells at any time during fermentation. The optimum phosphate concentration for alkaloid production by immobilized cells (about 0.5 mM) was a quarter of that required by free cells. This optimum shift was attributed to (i) the diminished phosphate demand of immobilized cells, due to their reduced metabolic activities, and (ii) the phosphate-dependent morphological behaviour of the biocatalyst. The observed decrease in alkaloid concentrations during later periods of the fermentation supported the idea of alkaloid-degradative enzymes, activated by high phosphate concentrations. Immobilization showed an advantageous influence on this undesirable effect.

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“…Since a distinction between certain lumi-EAs was not possible with this method, it showed the sum of all lumi-EAs in the sample. Later, lumi-ergotamine was detected in pharmaceutical preparations via HPLC-UV (Bethke et al 1976). The conversion of EAs to their lumi-compounds by post-column derivatization via a photochemical reactor was used by Scholten and Frei (1979).…”

Section: Introductionmentioning

confidence: 99%

Lumi-ergometrine – structural identification and occurrence in sclerotia

et al. 2011

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The fungus Claviceps purpurea grows on grasses and cereal grains and produces six predominant ergot alkaloids. These toxic substances undergo different transformation reactions during storage and cereal processing. One of these reactions is the addition of water to a double bond in the ergoline skeleton. Since light is required for this process, the substances formed were named lumi-ergot alkaloids. From these, a new asymmetric carbon and consequently two epimers with different polarities are formed. For investigations of lumi-ergot alkaloids, ergometrine was used exemplarily as it represents one of the six ergot alkaloids predominantly formed by Claviceps purpurea. The main reaction product, the less polar compound of the two lumi-ergometrine epimers, was separated by HPLC and unambiguously identified as 10-(S)-lumi-ergometrine using X-ray structural analysis. A HPLC-MS/MS method was developed for the detection of this substance in sclerotia extracts. Using this method, the existence of both epimeric forms of lumi-ergometrine could be proved in the sclerotia. This is the first time that the existence of a lumi-transformation product of ergot alkaloids was proved in naturally grown samples.

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Determination of the content and purity of ergotamine preparations by means of high-pressure liquid chromatography

Cited by 40 publications

References 6 publications

Determination of dihydroergocryptine in human plasma and urine samples using on-line sample extraction?column-switching reversed-phase liquid chromatography?mass spectrometry

Determination of dihydroergocryptine in human plasma and urine samples using on-line sample extraction?column-switching reversed-phase liquid chromatography?mass spectrometry

Influence of inorganic phosphate and immobilization on Claviceps purpurea

Lumi-ergometrine – structural identification and occurrence in sclerotia

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