Greener approaches in the extraction of the biological samples before the analysis of naltrexone and its major metabolite by HPLC


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Tok K. C., Bozmaoğlu H. C., Gümüştaş M., Süzen H. S.

32nd International Symposium on Pharmaceutical and Biomedical Analysis, Mons, Belçika, 11 - 14 Eylül 2022, ss.88

  • Yayın Türü: Bildiri / Özet Bildiri
  • Basıldığı Şehir: Mons
  • Basıldığı Ülke: Belçika
  • Sayfa Sayıları: ss.88
  • Ankara Üniversitesi Adresli: Evet

Özet

Naltrexone (NTX) is an opioid antagonist that blocks the pharmacologic effect of opioids such as morphine and heroin etc. It has highly efficacious blocking capability with competitive antagonist activity at µ-opioid receptors. It also undergoes extensive hepatic metabolism, primarily via the reduction of its major metabolite, 6-β naltrexol (6BNTX) (Figure 1). 6BNTX is believed to be a major contributor to the pharmacological effect of naltrexone.

This study aims to develop extraction methodologies for greener, more sensitive, reliable, and precise determination of NTX and its metabolite by using high-performance liquid chromatography (HPLC) followed by UV detection. Based on the literature survey there is a gap in sample preparation methods for these compounds. In the literature, mostly used extraction techniques from biological matrices were liquid-liquid extraction and solid-phase extraction. However, greener approaches need to be developed to reduce organic waste consumption. During the development of the dispersive liquid-liquid microextraction (DLLME) method, acetonitrile, acetone, and methanol were compared as dispersive solvents, chloroform, chlorobenzene, carbon tetrachloride, and carbon disulfide, 1,2 dichloroethane, and trichloroethylene were compared as extraction solvents. Furthermore, an investigation of the effects of ionic strength and pH on extraction efficiency was realized. Optimized conditions for the extraction methodology were used to analyse both compounds simultaneously from biological media by using Kinetex EVO C18 (150 mm x 4.6 mm i.d., 2.6 μm) as an analytical column. The optimized HPLC-UV methodology was validated according to the International Council for Harmonization Guidelines in terms of selectivity, linearity, range, the limit of detection and quantification, accuracy, precision, etc.