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