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Description
  • Estrogen steroids, represented by estradiol and its related substances, include both structurally very close and simultaneously different analogs. Their separation still remains an analytical challenge. Subcritical fluid chromatography (SbFC) on sub-2-micron particles was found to be an appropriate tool to obtain fast and efficient separation of nine target analytes. Among the four tested stationary phases charged hybrid modified with PFP (pentafluorophenyl) moiety was found to be the most convenient providing the fastest separation within 1.6 min using quick gradient elution with carbon dioxide and methanol as an organic modifier. However, complete separation was obtained also on other tested phases including bare hybrid stationary phase, hybrid stationary phase modified with 2-EP (2-ethylpyridine) and also 08, which is less typical in SbFC. The baseline separation on the latter columns was achieved by means of a temperature increase, a change in organic modifier type and gradient time increase respectively. Quantitative performance was evaluated at optimized conditions and method validation was accomplished. Excellent repeatability of both retention times (RSD <0.15%) and peak areas (RSD < 1%) was observed. The method was linear in the range of 1.0-1000.0 mu g/ml for all steroids with the lowest calibration point being an LOQ except for Delta-derivatives, that provided better sensitivity and thus LOQ of 0.5 mu g/ml. The sensitivity was sufficient for the analysis of real samples although it was still five times lower compared to UHPLC-UV experiments.
  • Estrogen steroids, represented by estradiol and its related substances, include both structurally very close and simultaneously different analogs. Their separation still remains an analytical challenge. Subcritical fluid chromatography (SbFC) on sub-2-micron particles was found to be an appropriate tool to obtain fast and efficient separation of nine target analytes. Among the four tested stationary phases charged hybrid modified with PFP (pentafluorophenyl) moiety was found to be the most convenient providing the fastest separation within 1.6 min using quick gradient elution with carbon dioxide and methanol as an organic modifier. However, complete separation was obtained also on other tested phases including bare hybrid stationary phase, hybrid stationary phase modified with 2-EP (2-ethylpyridine) and also 08, which is less typical in SbFC. The baseline separation on the latter columns was achieved by means of a temperature increase, a change in organic modifier type and gradient time increase respectively. Quantitative performance was evaluated at optimized conditions and method validation was accomplished. Excellent repeatability of both retention times (RSD <0.15%) and peak areas (RSD < 1%) was observed. The method was linear in the range of 1.0-1000.0 mu g/ml for all steroids with the lowest calibration point being an LOQ except for Delta-derivatives, that provided better sensitivity and thus LOQ of 0.5 mu g/ml. The sensitivity was sufficient for the analysis of real samples although it was still five times lower compared to UHPLC-UV experiments. (en)
Title
  • Ultra-fast separation of estrogen steroids using subcritical fluid chromatography on sub-2-micron particles
  • Ultra-fast separation of estrogen steroids using subcritical fluid chromatography on sub-2-micron particles (en)
skos:prefLabel
  • Ultra-fast separation of estrogen steroids using subcritical fluid chromatography on sub-2-micron particles
  • Ultra-fast separation of estrogen steroids using subcritical fluid chromatography on sub-2-micron particles (en)
skos:notation
  • RIV/00216208:11160/14:10282197!RIV15-MSM-11160___
http://linked.open...avai/riv/aktivita
http://linked.open...avai/riv/aktivity
  • I
http://linked.open...iv/cisloPeriodika
  • April
http://linked.open...vai/riv/dodaniDat
http://linked.open...aciTvurceVysledku
http://linked.open.../riv/druhVysledku
http://linked.open...iv/duvernostUdaju
http://linked.open...titaPredkladatele
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  • 51783
http://linked.open...ai/riv/idVysledku
  • RIV/00216208:11160/14:10282197
http://linked.open...riv/jazykVysledku
http://linked.open.../riv/klicovaSlova
  • Method development; Sub-2-micron particles; Subcritical fluid chromatography; Estrogens; Steroids (en)
http://linked.open.../riv/klicoveSlovo
http://linked.open...odStatuVydavatele
  • GB - Spojené království Velké Británie a Severního Irska
http://linked.open...ontrolniKodProRIV
  • [CB1599488E38]
http://linked.open...i/riv/nazevZdroje
  • Talanta
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http://linked.open...ichTvurcuVysledku
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http://linked.open...UplatneniVysledku
http://linked.open...v/svazekPeriodika
  • 121
http://linked.open...iv/tvurceVysledku
  • Solich, Petr
  • Nováková, Lucie
  • Chocholouš, Petr
http://linked.open...ain/vavai/riv/wos
  • 000333791500023
issn
  • 0039-9140
number of pages
http://bibframe.org/vocab/doi
  • 10.1016/j.talanta.2013.12.056
http://localhost/t...ganizacniJednotka
  • 11160
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