Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV
A sensitive, precise, accurate, and specific isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous separation and determination of zolmitriptan, naratriptan, dihydroergotamine, ketotifen, and pizotifen in pharmaceutical formulations has been developed...
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| Format: | Article |
| Language: | English |
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Wiley
2019-01-01
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| Series: | International Journal of Analytical Chemistry |
| Online Access: | http://dx.doi.org/10.1155/2019/9685750 |
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| author | Sami Jebali Chaouki Belgacem Mohamed Radhouen Louhaichi Senda Bahri Latifa Latrous El Atarche |
| author_facet | Sami Jebali Chaouki Belgacem Mohamed Radhouen Louhaichi Senda Bahri Latifa Latrous El Atarche |
| author_sort | Sami Jebali |
| collection | DOAJ |
| description | A sensitive, precise, accurate, and specific isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous separation and determination of zolmitriptan, naratriptan, dihydroergotamine, ketotifen, and pizotifen in pharmaceutical formulations has been developed and validated. An experimental design was applied for the optimization of the chromatographic parameters. A two-level full factorial 2k was used for studying the interaction between the variables to be optimized: the percentage of acetonitrile in the mobile phase, mobile-phase pH, nature of the buffer, and column oven temperature. The most significant parameters are the percentage of acetonitrile and the mobile-phase pH. These significant parameters were optimized using the Doehlert matrix. The optimum separation was achieved by means of a Waters XBridge C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of acetonitrile and a 10 mM sodium perchlorate buffer (38 : 62, v/v) at a flow rate of 1.0 mL·min−1 and UV detection at 220 nm. The selectivity, method linearity, accuracy, and precision were examined as part of the method validation. The described method shows excellent linearity over a range of 30 to 70 μg·mL−1 for all compounds with correlation coefficients higher than 0.995. The standard deviations of the intraday and interday precision were between 0.75 and 1.94%. The validated method was successfully applied to perform routine analysis of these compounds in different pharmaceutical products such as syrups and tablets. In the presence of some preservatives, it was found that there were no peaks at the related peak locations. |
| format | Article |
| id | doaj-art-2df91b3ee7ff4ff4bcf54ffbbd925f9c |
| institution | Kabale University |
| issn | 1687-8760 1687-8779 |
| language | English |
| publishDate | 2019-01-01 |
| publisher | Wiley |
| record_format | Article |
| series | International Journal of Analytical Chemistry |
| spelling | doaj-art-2df91b3ee7ff4ff4bcf54ffbbd925f9c2025-02-03T05:53:41ZengWileyInternational Journal of Analytical Chemistry1687-87601687-87792019-01-01201910.1155/2019/96857509685750Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UVSami Jebali0Chaouki Belgacem1Mohamed Radhouen Louhaichi2Senda Bahri3Latifa Latrous El Atarche4Laboratoire National de Contrôle des Médicaments, 11 Bis Rue Jebel Lakhdar Bab Saadoun, 1006 Tunis, TunisiaUniversité de Tunis El Manar, Faculté des Sciences de Tunis, Laboratoire de Chimie Analytique et Electrochimie, Campus Universitaire El Manar II 2092, Tunis, TunisiaLaboratoire National de Contrôle des Médicaments, 11 Bis Rue Jebel Lakhdar Bab Saadoun, 1006 Tunis, TunisiaLaboratoire National de Contrôle des Médicaments, 11 Bis Rue Jebel Lakhdar Bab Saadoun, 1006 Tunis, TunisiaUniversité de Tunis El Manar, Faculté des Sciences de Tunis, Laboratoire de Chimie Analytique et Electrochimie, Campus Universitaire El Manar II 2092, Tunis, TunisiaA sensitive, precise, accurate, and specific isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous separation and determination of zolmitriptan, naratriptan, dihydroergotamine, ketotifen, and pizotifen in pharmaceutical formulations has been developed and validated. An experimental design was applied for the optimization of the chromatographic parameters. A two-level full factorial 2k was used for studying the interaction between the variables to be optimized: the percentage of acetonitrile in the mobile phase, mobile-phase pH, nature of the buffer, and column oven temperature. The most significant parameters are the percentage of acetonitrile and the mobile-phase pH. These significant parameters were optimized using the Doehlert matrix. The optimum separation was achieved by means of a Waters XBridge C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of acetonitrile and a 10 mM sodium perchlorate buffer (38 : 62, v/v) at a flow rate of 1.0 mL·min−1 and UV detection at 220 nm. The selectivity, method linearity, accuracy, and precision were examined as part of the method validation. The described method shows excellent linearity over a range of 30 to 70 μg·mL−1 for all compounds with correlation coefficients higher than 0.995. The standard deviations of the intraday and interday precision were between 0.75 and 1.94%. The validated method was successfully applied to perform routine analysis of these compounds in different pharmaceutical products such as syrups and tablets. In the presence of some preservatives, it was found that there were no peaks at the related peak locations.http://dx.doi.org/10.1155/2019/9685750 |
| spellingShingle | Sami Jebali Chaouki Belgacem Mohamed Radhouen Louhaichi Senda Bahri Latifa Latrous El Atarche Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV International Journal of Analytical Chemistry |
| title | Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV |
| title_full | Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV |
| title_fullStr | Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV |
| title_full_unstemmed | Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV |
| title_short | Application of Factorial and Doehlert Designs for the Optimization of the Simultaneous Separation and Determination of Antimigraine Drugs in Pharmaceutical Formulations by RP-HPLC-UV |
| title_sort | application of factorial and doehlert designs for the optimization of the simultaneous separation and determination of antimigraine drugs in pharmaceutical formulations by rp hplc uv |
| url | http://dx.doi.org/10.1155/2019/9685750 |
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