Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements

Jing Li, Si Hun Roh, Jia Shaodong, Ji Yeon Hong, Dong Kyu Lee, Byong kyu Shin, Jeong Hill Park, Jeongmi Lee, Sung Won Kwon

Research output: Contribution to journalArticle

3 Scopus citations

Abstract

A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements.

Original languageEnglish (US)
JournalJournal of Separation Science
DOIs
StateAccepted/In press - 2017

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Keywords

  • Adulteration
  • Ion-pairing chromatography
  • Mixed-mode solid-phase extraction
  • Reversed-phase dispersive liquid-liquid microextraction
  • Sildenafil

ASJC Scopus subject areas

  • Analytical Chemistry
  • Filtration and Separation

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