Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol
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 beha...
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| Format: | Article |
| Language: | English |
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Sciendo
2018-12-01
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| Series: | Acta Pharmaceutica |
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| Online Access: | https://doi.org/10.2478/acph-2018-0036 |
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| author | Shehzadi Naureen Hussain Khalid Islam Muhammad Bukhari Nadeem Irfan Khan Muhammad Tanveer Salman Muhammad Siddiqui Sabahat Zahra Rehman Aziz-Ur Abbasi Muhammad Athar |
| author_facet | Shehzadi Naureen Hussain Khalid Islam Muhammad Bukhari Nadeem Irfan Khan Muhammad Tanveer Salman Muhammad Siddiqui Sabahat Zahra Rehman Aziz-Ur Abbasi Muhammad Athar |
| author_sort | Shehzadi Naureen |
| collection | DOAJ |
| description | 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 that 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 might be a result of N- or Smethylation 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. |
| format | Article |
| id | doaj-art-a365c901889243b3ae406057705fbc02 |
| institution | Kabale University |
| issn | 1846-9558 |
| language | English |
| publishDate | 2018-12-01 |
| publisher | Sciendo |
| record_format | Article |
| series | Acta Pharmaceutica |
| spelling | doaj-art-a365c901889243b3ae406057705fbc022025-02-02T17:46:44ZengSciendoActa Pharmaceutica1846-95582018-12-0168440942410.2478/acph-2018-0036acph-2018-0036Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-ThiolShehzadi Naureen0Hussain Khalid1Islam Muhammad2Bukhari Nadeem Irfan3Khan Muhammad Tanveer4Salman Muhammad5Siddiqui Sabahat Zahra6Rehman Aziz-Ur7Abbasi Muhammad Athar8Punjab University College of Pharmacy, University of the Punjab Allama Iqbal Campus, Lahore-54030,Lahore, PakistanPunjab University College of Pharmacy, University of the Punjab Allama Iqbal Campus, Lahore-54030Lahore, PakistanPunjab University College of Pharmacy, University of the Punjab Allama Iqbal Campus, Lahore-54030Lahore, PakistanPunjab University College of Pharmacy, University of the Punjab Allama Iqbal Campus, Lahore-54030Lahore, PakistanFaculty of Pharmacy, University of Lahore,Lahore, PakistanPunjab University College of Pharmacy, University of the Punjab Allama Iqbal Campus, Lahore-54030Lahore, PakistanDepartment of Chemistry Government College University Lahore-54030,Lahore, PakistanDepartment of Chemistry Government College University Lahore-54030,Lahore, PakistanDepartment of Chemistry Government College University Lahore-54030,Lahore, PakistanThe 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 that 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 might be a result of N- or Smethylation 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.https://doi.org/10.2478/acph-2018-00365-[(4-chlorophenoxy)methyl]-1,3,4-oxadiazole-2-thiolforced degradationstabilityrp-hplc/dad |
| spellingShingle | Shehzadi Naureen Hussain Khalid Islam Muhammad Bukhari Nadeem Irfan Khan Muhammad Tanveer Salman Muhammad Siddiqui Sabahat Zahra Rehman Aziz-Ur Abbasi Muhammad Athar Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol Acta Pharmaceutica 5-[(4-chlorophenoxy)methyl]-1,3,4-oxadiazole-2-thiol forced degradation stability rp-hplc/dad |
| title | Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol |
| title_full | Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol |
| title_fullStr | Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol |
| title_full_unstemmed | Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol |
| title_short | Reverse-Phase Chromatographic Determination and Intrinsic Stability Behavior of 5-[(4-Chlorophenoxy)Methyl]-1,3,4-Oxadiazole-2-Thiol |
| title_sort | reverse phase chromatographic determination and intrinsic stability behavior of 5 4 chlorophenoxy methyl 1 3 4 oxadiazole 2 thiol |
| topic | 5-[(4-chlorophenoxy)methyl]-1,3,4-oxadiazole-2-thiol forced degradation stability rp-hplc/dad |
| url | https://doi.org/10.2478/acph-2018-0036 |
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