Izvorni znanstveni članak

https://doi.org/10.2478/acph-2018-0036

Reverse-phase chromatographic determination and intrinsic stability behavior of 5-[(4-chlorophenoxy)methyl]-1,3,4-oxadiazole-2-thiol

NAUREEN SHEHZADI ; Punjab University College of Pharmacy, University of the Punjab, Allama Iqbal Campus, Lahore-54030, Pakistan
KHALID HUSSAIN ; Punjab University College of Pharmacy, University of the Punjab, Allama Iqbal Campus, Lahore-54030, Pakistan
MUHAMMAD ISLAM ; Punjab University College of Pharmacy, University of the Punjab, Allama Iqbal Campus, Lahore-54030, Pakistan; Faculty of Pharmacy, the University of Lahore, Lahore, Pakistan
NADEEM IRFAN BUKHARI ; Punjab University College of Pharmacy, University of the Punjab, Allama Iqbal Campus, Lahore-54030, Pakistan
MUHAMMAD TANVEER KHAN ; Faculty of Pharmacy, the University of Lahore, Lahore, Pakistan
MUHAMMAD SALMAN ; Punjab University College of Pharmacy, University of the Punjab, Allama Iqbal Campus, Lahore-54030, Pakistan
SABAHAT ZAHRA SIDDIQUI ; Department of Chemistry, Government College University, Lahore-54030, Pakistan
AZIZ-UR REHMAN ; Department of Chemistry, Government College University, Lahore-54030, Pakistan
MUHAMMAD ATHAR ABBASI ; Department of Chemistry, Government College University, Lahore-54030, Pakistan

Sažetak

The study describes the development and preliminary validation of a simple reverse phase chromatographic method for determination of a novel drug candidate, 5-[(4-chlorophenoxy)methyl]-1,3,4-oxadiazole-2-thiol (OXCPM), in bulk and stressed solution, in order to find out the intrinsic stability behavior of the compound. Isocratic elution was carried out at a flow rate of 1.0 mL min–1 through a Promosil C18 column maintained at 25 °C, using the mobile phase comprising acetonitrile and aqueous o-H3PO4 (pH 2.67) (1:1, V/V). Detection was performed at 258 nm. The response of the detector was linear in a concentration range of 1.25–50.00 µg mL–1 with the correlation coefficient of 0.9996 ± 0.0001. Cumulative intra-day, inter-day and inter-instrument accuracy (99.5 ± 1.0, 100.2 ± 1.0 and 100.3 ± 0.4 %, resp.) with RSD less than 5 % indicated that the method was accurate and precise. The resolution and selectivity factor (>2 and >1, resp.), particularly in copper metal- and dry-heat-stress solutions, depicted the selectivity of the method. OXCPM remained stable under hydrolytic (acidic and neutral pH, ≤ 37 °C), photolytic and moist heat stress conditions. Under alkaline conditions (hydrolytic and photolytic), polar products were formed and eluted very fast through the column (tR < 3.75 min). At room temperature, the compound was susceptible to oxidation by hydrogen peroxide and transition metals. The ionogram of most of the stress solutions indicated the presence of a product having m/z 256, which may be a result of N- or S- methylation or -SH oxidation. The results of the study indicate that the method is selective, sensitive and suitable to be used for determination of OXCPM in bulk and under stress conditions.

Ključne riječi

5-[(4-chlorophenoxy) methyl]-1,3,4-oxadiazole-2-thiol; forced degradation; stability; RP-HPLC/DAD

Hrčak ID:

202261

URI

https://hrcak.srce.hr/202261

Datum izdavanja:

31.12.2018.

Posjeta: 854 *