Determination of sibiromycin and its natural derivatives using new analytical and structural approaches

作者：Sulc Miroslav; Fadrhoncova Iva; Jelinkova Marketa; Chudomelova Miriam; Fel**erg Juergen; Olsovska Jana^*

来源：Journal of Chromatography A, 2011, 1218(1): 83-91.

DOI：10.1016/j.chroma.2010.10.110

• Sibiromycin
• UHPLC
• Mass spectrometry
• Solid phase extraction

A new separation and quantification method using ultra high-performance liquid chromatography (UHPLC) with UV detection was developed for the detection of sibiromycin in fermentation broth of Streptosporangium sibiricum. The solid phase extraction method based on cation-exchange was employed to pre-concentrate and purify fermentation broth containing sibiromycin prior to UHPLC analysis. The whole assay was validated and showed a linear range of detector response for the quantification of sibiromycin in a concentration from 3.9 to 250.0 mu g mL(-1), with correlation coefficient of 0.999 and recoveries ranging from 71.66 +/- 3.55% to 74.76 +/- 5.18%. Method limit of quantification of the assay was determined as 0.18 mu g mL(-1) and was verified with resulting RSD of 9.6% and accuracy of 97.6%. The developed assay was used to determine the sibiromycin production in 12 different fermentation broths. Moreover, several natural sibiromycin analogues/derivatives were described with pilot characterization using off-line mass spectrometry: the previously described dihydro-sibiromycin (DH-sibiromycin) and tentative bis-glycosyl forms of sibiromycin and its dihydro-analogue.

• 出版日期2011-1-7