DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT
We developed and validated a stability-indicating method for the simultaneous determination of allopurinol and ketoconazole in the pharmaceutical form of capsules. A Dionex® liquid chromatograph equipped with a diode array detector (DAD) and InertSustain® C18 column (4.6 x 100 mm x 3 μm) was used an...
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| Format: | Article |
| Language: | English |
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Universidade Federal do Rio Grande do Sul
2020-12-01
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| Series: | Drug Analytical Research |
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| Online Access: | https://seer.ufrgs.br/dar/article/view/102740/59387 |
| _version_ | 1818927534779138048 |
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| author | Patrícia Espinosa dos Santos Ana Carla Lucca Marcos Serrou do Amaral Nájla Mohamad Kassab |
| author_facet | Patrícia Espinosa dos Santos Ana Carla Lucca Marcos Serrou do Amaral Nájla Mohamad Kassab |
| author_sort | Patrícia Espinosa dos Santos |
| collection | DOAJ |
| description | We developed and validated a stability-indicating method for the simultaneous determination of allopurinol and ketoconazole in the pharmaceutical form of capsules. A Dionex® liquid chromatograph equipped with a diode array detector (DAD) and InertSustain® C18 column (4.6 x 100 mm x 3 μm) was used and InertSustain® C18 column (4.6 x 100 mm x 3 μm). The chromatographic separation occurred in the isocratic mode with a flow rate of 0.45 mL min-1 and mobile phase composed of acetonitrile: water (52:48 v/v) with pH adjusted to 3.0. The wavelengths used were 250 nm for allopurinol and 225 nm for ketoconazole. The method was validated by evaluating the parameters of linearity, limits of detection and quantification, precision, accuracy, robustness, and selectivity. The method presented linearity. It was precise, with coefficients of variation lower than 2.0%, and accurate, with recovery close to 100.00%. Robustness was indicated by the Plackett-Burman model, and the method was not significantly influenced by any of the variations. The selectivity was proven by the peak purities close to 1000 in both the presence of excipients and drug degradation products. Therefore the proposed method is simple and fast, with separation for both drugs less than four minutes. |
| first_indexed | 2024-12-20T03:14:33Z |
| format | Article |
| id | doaj.art-9fd05e08e6194b2aaf931119f9627832 |
| institution | Directory Open Access Journal |
| issn | 2527-2616 |
| language | English |
| last_indexed | 2024-12-20T03:14:33Z |
| publishDate | 2020-12-01 |
| publisher | Universidade Federal do Rio Grande do Sul |
| record_format | Article |
| series | Drug Analytical Research |
| spelling | doaj.art-9fd05e08e6194b2aaf931119f96278322022-12-21T19:55:23ZengUniversidade Federal do Rio Grande do SulDrug Analytical Research2527-26162020-12-01422430https://doi.org/10.22456/2527-2616.102740DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENTPatrícia Espinosa dos Santos0https://orcid.org/0000-0001-7142-0297Ana Carla Lucca1Marcos Serrou do Amaral2https://orcid.org/0000-0001-8101-6933Nájla Mohamad Kassab3https://orcid.org/0000-0002-9324-4252Universidade Federal de Mato Grosso do SulUniversidade Federal de Mato Grosso do SulUniversidade Federal de Mato Grosso do SulUniversidade Federal de Mato Grosso do SulWe developed and validated a stability-indicating method for the simultaneous determination of allopurinol and ketoconazole in the pharmaceutical form of capsules. A Dionex® liquid chromatograph equipped with a diode array detector (DAD) and InertSustain® C18 column (4.6 x 100 mm x 3 μm) was used and InertSustain® C18 column (4.6 x 100 mm x 3 μm). The chromatographic separation occurred in the isocratic mode with a flow rate of 0.45 mL min-1 and mobile phase composed of acetonitrile: water (52:48 v/v) with pH adjusted to 3.0. The wavelengths used were 250 nm for allopurinol and 225 nm for ketoconazole. The method was validated by evaluating the parameters of linearity, limits of detection and quantification, precision, accuracy, robustness, and selectivity. The method presented linearity. It was precise, with coefficients of variation lower than 2.0%, and accurate, with recovery close to 100.00%. Robustness was indicated by the Plackett-Burman model, and the method was not significantly influenced by any of the variations. The selectivity was proven by the peak purities close to 1000 in both the presence of excipients and drug degradation products. Therefore the proposed method is simple and fast, with separation for both drugs less than four minutes.https://seer.ufrgs.br/dar/article/view/102740/59387allopurinolketoconazolecanine visceral leishmaniasisanalytical validationliquid chromatography |
| spellingShingle | Patrícia Espinosa dos Santos Ana Carla Lucca Marcos Serrou do Amaral Nájla Mohamad Kassab DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT Drug Analytical Research allopurinol ketoconazole canine visceral leishmaniasis analytical validation liquid chromatography |
| title | DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT |
| title_full | DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT |
| title_fullStr | DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT |
| title_full_unstemmed | DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT |
| title_short | DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ANALYTICAL METHOD FOR SIMULTANEOUS DETERMINATION OF DRUGS EMPLOYED IN CANINE LEISHMANIASIS TREATMENT |
| title_sort | development and validation of a stability indicating analytical method for simultaneous determination of drugs employed in canine leishmaniasis treatment |
| topic | allopurinol ketoconazole canine visceral leishmaniasis analytical validation liquid chromatography |
| url | https://seer.ufrgs.br/dar/article/view/102740/59387 |
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