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Muzashvili T.,Institute of Pharmacochemistry | Perrone A.,University of Salerno | Napolitano A.,University of Salerno | Kemertelidze E.,Institute of Pharmacochemistry | And 2 more authors.
Phytochemistry | Year: 2011

Nine furostanol glycosides, namely caucasicosides E-M, were isolated from the MeOH extract of the leaves of Helleborus caucasicus, along with 11 known compounds including nine furostanol glycosides, a bufadienolide and an ecdysteroid. Their structures were established by the extensive use of 1D and 2D NMR experiments along with ESIMS n analyses. The steroidal composition of leaves of H. caucasicus shows as particular feature the occurrence of steroidal compounds belonging to the 5β series, unusual for Helleborus species, and in particular, caucasicosides F-H are based on a 5β-polyhydroxylated steroidal aglycon never reported before. © 2011 Elsevier Ltd. All rights reserved.

Napolitano A.,University of Salerno | Muzashvili T.,Institute of Pharmacochemistry | Perrone A.,University of Salerno | Pizza C.,University of Salerno | And 2 more authors.
Phytochemistry | Year: 2011

A comparative metabolite profiling of the underground parts and leaves of Ruscus ponticus was obtained by an HPLC-ESIMSn method, based on high-performance liquid chromatography coupled to electrospray positive ionization multistage ion trap mass spectrometry. The careful study of HPLC-ESIMSn fragmentation pattern of each chromatographic peak, in particular the identification of diagnostic product ions, allowed us to get a rapid screening of saponins belonging to different classes, such as dehydrated/or not furostanol, spirostanol and pregnane glycosides, and to promptly highlight similarities and differences between the two plant parts. This approach, followed by isolation and structure elucidation by 1D- and 2D-NMR experiments, led to the identification of eleven saponins from the underground parts, of which two dehydrated furostanol glycosides and one new vespertilin derivative, and nine saponins from R. ponticus leaves, never reported previously. The achieved results highlighted a clean prevalence of furostanol glycoside derivatives in R. ponticus leaves rather in the underground parts of the plant, which showed a wider structure variety. In particular, the occurrence of dehydrated furostanol derivatives, for the first time isolated from a Ruscus species, is an unusual finding which makes unique the saponins profile of R. ponticus. © 2011 Elsevier Ltd. All rights reserved.

Montoro P.,University of Salerno | Skhirtladze A.,Institute of Pharmacochemistry | Perrone A.,University of Salerno | Benidze M.,Institute of Pharmacochemistry | And 2 more authors.
Journal of Pharmaceutical and Biomedical Analysis | Year: 2010

An high-performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS) method, was developed for the quantitative analysis of the steroidal glycosides occurring in Yucca gloriosa flowers. The HPLC experiments were performed by means of an octadecyl-modified reversed-phase C-18 column and a binary mobile phase system under gradient elution conditions. The fragmentation patterns of steroidal saponins were analyzed by ESI-MSn in positive ion mode and a specific multiple reaction monitoring MS/MS detection was developed for their quantitative determination. The described method provides high sensitivity and specificity for quantitative determination of the steroidal glycosides in Y. gloriosa flowers. Quantification was performed against an external calibration line obtained using each pure steroidal glycoside. Short- and long-term repeatabilities of the methods were better than 3 and 6%, respectively. The method was validated according to EMEA guidelines and applied to real samples. © 2010 Elsevier B.V.

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