Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment
Cefoperazone (CPZ) is a third-generation cephalosporin used to treat bovine mastitis. The association with steroidal anti-inflammatory drugs, such as prednisolone (PRED), provides an improvement in the animal's clinical response, which justifies its use. An analytical method capable of simultan...
Saved in:
| Main Authors: | , , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
Universidade Federal do Rio Grande do Sul
2025-07-01
|
| Series: | Drug Analytical Research |
| Subjects: | |
| Online Access: | https://seer.ufrgs.br/index.php/dar/article/view/146375/96052 |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| _version_ | 1850060532273381376 |
|---|---|
| author | Patrícia Espinosa dos Santos Jefferson Annunciatto Teófilo Fernando Mazon Cardoso Marcos Serrou do Amaral Nájla Mohamad Kassab |
| author_facet | Patrícia Espinosa dos Santos Jefferson Annunciatto Teófilo Fernando Mazon Cardoso Marcos Serrou do Amaral Nájla Mohamad Kassab |
| author_sort | Patrícia Espinosa dos Santos |
| collection | DOAJ |
| description | Cefoperazone (CPZ) is a third-generation cephalosporin used to treat bovine mastitis. The association with steroidal anti-inflammatory drugs, such as prednisolone (PRED), provides an improvement in the animal's clinical response, which justifies its use. An analytical method capable of simultaneously determining the association between CPZ and PRED by High Performance Liquid Chromatography coupled with a Diode Array Detector (HPLC-DAD) was developed. The method was applied in intramammary ointments, showing linearity, for CPZ, from 0.25 to 25 μg mL-1 (r=0.9999); and, for PRED, from 0.75 to 30 μg mL-1 (r=0.9997), with low limits of detection and quantification, precision with coefficients of variation less than 2%, in accuracy, presented recovery close to 100% for both drugs, in addition to demonstrating their robustness by the Youden test, which evaluated the effects and concluded that the altered parameters in the test were not sufficient to change the values obtained in the determinations. The test was also applied to the commercial sample for quality control purposes, with extraction efficiency being 69.66% for CPZ and 72.36% for PRED. Thus, the developed and validated method can be safely applied in the analysis of the studied drugs. |
| format | Article |
| id | doaj-art-2d5349121ae0477781f35d6d6b9be342 |
| institution | DOAJ |
| issn | 2527-2616 |
| language | English |
| publishDate | 2025-07-01 |
| publisher | Universidade Federal do Rio Grande do Sul |
| record_format | Article |
| series | Drug Analytical Research |
| spelling | doaj-art-2d5349121ae0477781f35d6d6b9be3422025-08-20T02:50:32ZengUniversidade Federal do Rio Grande do SulDrug Analytical Research2527-26162025-07-01910312https://doi.org/10.22456/2527-2616.146375Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointmentPatrícia Espinosa dos Santos0https://orcid.org/0000-0001-7142-0297Jefferson Annunciatto1https://orcid.org/0009-0007-8295-6311Teófilo Fernando Mazon Cardoso2https://orcid.org/0000-0001-7392-7366Marcos Serrou do Amaral3https://orcid.org/0000-0001-8101-6933Nájla Mohamad Kassab4https://orcid.org/0000-0002-9324-4252Laboratory of Pharmaceutical Technology, Faculty of Pharmaceutical Sciences, Food, and Nutrition, Federal University of Mato Grosso do Sul, Campo Grande, MS, BrazilPrograma de Pós-Graduação em Ciências Farmacêuticas; Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande (MS), BrasilFaculdade de Ciências Farmacêuticas, Alimentos e Nutrição, Universidade Federal de Mato Grosso do Sul (UFMS)Instituto de Física, Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande (MS), BrasilFaculdade de Ciências Farmacêuticas, Alimentos e Nutrição, Universidade Federal de Mato Grosso do Sul (UFMS)Cefoperazone (CPZ) is a third-generation cephalosporin used to treat bovine mastitis. The association with steroidal anti-inflammatory drugs, such as prednisolone (PRED), provides an improvement in the animal's clinical response, which justifies its use. An analytical method capable of simultaneously determining the association between CPZ and PRED by High Performance Liquid Chromatography coupled with a Diode Array Detector (HPLC-DAD) was developed. The method was applied in intramammary ointments, showing linearity, for CPZ, from 0.25 to 25 μg mL-1 (r=0.9999); and, for PRED, from 0.75 to 30 μg mL-1 (r=0.9997), with low limits of detection and quantification, precision with coefficients of variation less than 2%, in accuracy, presented recovery close to 100% for both drugs, in addition to demonstrating their robustness by the Youden test, which evaluated the effects and concluded that the altered parameters in the test were not sufficient to change the values obtained in the determinations. The test was also applied to the commercial sample for quality control purposes, with extraction efficiency being 69.66% for CPZ and 72.36% for PRED. Thus, the developed and validated method can be safely applied in the analysis of the studied drugs.https://seer.ufrgs.br/index.php/dar/article/view/146375/96052cefoperazoneprednisolonevalidationhplcquality control |
| spellingShingle | Patrícia Espinosa dos Santos Jefferson Annunciatto Teófilo Fernando Mazon Cardoso Marcos Serrou do Amaral Nájla Mohamad Kassab Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment Drug Analytical Research cefoperazone prednisolone validation hplc quality control |
| title | Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| title_full | Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| title_fullStr | Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| title_full_unstemmed | Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| title_short | Development and validation of an HPLC-DAD analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| title_sort | development and validation of an hplc dad analytical method for quantitative and simultaneous determination of cefoperazone and prednisolone in intramammary ointment |
| topic | cefoperazone prednisolone validation hplc quality control |
| url | https://seer.ufrgs.br/index.php/dar/article/view/146375/96052 |
| work_keys_str_mv | AT patriciaespinosadossantos developmentandvalidationofanhplcdadanalyticalmethodforquantitativeandsimultaneousdeterminationofcefoperazoneandprednisoloneinintramammaryointment AT jeffersonannunciatto developmentandvalidationofanhplcdadanalyticalmethodforquantitativeandsimultaneousdeterminationofcefoperazoneandprednisoloneinintramammaryointment AT teofilofernandomazoncardoso developmentandvalidationofanhplcdadanalyticalmethodforquantitativeandsimultaneousdeterminationofcefoperazoneandprednisoloneinintramammaryointment AT marcosserroudoamaral developmentandvalidationofanhplcdadanalyticalmethodforquantitativeandsimultaneousdeterminationofcefoperazoneandprednisoloneinintramammaryointment AT najlamohamadkassab developmentandvalidationofanhplcdadanalyticalmethodforquantitativeandsimultaneousdeterminationofcefoperazoneandprednisoloneinintramammaryointment |