A new magnetic nanodiamond/graphene oxide hybrid (Fe3O4@ND@GO) material for pre-concentration and sensitive determination of sildenafil in alleged herbal aphrodisiacs by HPLC-DAD system


YILMAZ E., ULUSOY H. İ., Demir O., SOYLAK M.

JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, cilt.1084, ss.113-121, 2018 (SCI-Expanded) identifier identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 1084
  • Basım Tarihi: 2018
  • Doi Numarası: 10.1016/j.jchromb.2018.03.030
  • Dergi Adı: JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.113-121
  • Anahtar Kelimeler: Sildenafil citrate, Magnetic hybrid material, Magnetic solid phase extraction, Grapheme oxide, Nanodiamond, High performance liquid chromatography, Herbal products, SOLID-PHASE EXTRACTION, ABSORPTION SPECTROMETRIC DETERMINATIONS, DOPED DIAMOND ELECTRODE, CITRATE VIAGRA, DIETARY-SUPPLEMENTS, PHARMACEUTICAL FORMULATIONS, MASS-SPECTROMETRY, WATER SAMPLES, ESI-MS, PRODUCTS
  • Sivas Cumhuriyet Üniversitesi Adresli: Evet

Özet

A sensitive analytical methodology was investigated to concentrate and determine of sildenafil citrate (SLC) present at trace level in herbal supplementary products. The proposed method is based on simple and sensitive pre-concentration of SLC by using magnetic solid phase extraction with new developed magnetic nanodiamond/graphene oxide hybrid (Fe3O4@ND@GO) material as a sorbent. Experimental variables affecting the extraction efficiency of SLC like; pH, sample volume, eluent type and volume, extraction time and amount of adsorbent were studied and optimized in detail. Determination of sildenafil citrate after magnetic solid phase extraction (MSPE) was carried out by HPLC-DAD system. The morphology, composition, and properties of the synthesized hybrid material was characterized by Fourier transform infrared spectrometry (FT-IR), Raman spectrometry (Raman), X-ray diffracdon spectrometry (XRD), scanning electron microscopy (SEM), mapping photographs, zeta potential analyzer, and BET surface area analysis. Under optimized conditions, linear range was ranged from 5.00 to 250.00 ng mL(-1) with R-2 of 0.9952. The limit of detection (LOD) was 1.49 ng mL(-1) and the recoveries at two spiked levels were ranged from 94.0 to 104.1% with the relative standard deviation (RSD) < 7.1% (n = 5). The enhancement factor (EF) was 86.9. The results show that the combination MSPE with HPLC-DAD is a suitable and sensitive method for the determination of SLC in real samples.