Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology
A combination of antibiotics and antiprotozoal and antisecretory medicines has been prescribed for the treatment of diarrhea. A rapid, reproducible liquid chromatographic procedure was established for the concurrent analysis of metronidazole (MET), ofloxacin (OFL), and racecadotril (RAC) in suspensi...
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2022-04-01
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| author | Mahesh Attimarad Katharigatta Narayanaswamy Venugopala Muhammad S. Chohan Pottathil Shinu Marysheela David Effren II Plaza Molina Anroop Balachandran Nair Nagaraja Sreeharsha Abdulrahman Ibrahim Altaysan Abdulmalek Ahmed Balgoname |
| author_facet | Mahesh Attimarad Katharigatta Narayanaswamy Venugopala Muhammad S. Chohan Pottathil Shinu Marysheela David Effren II Plaza Molina Anroop Balachandran Nair Nagaraja Sreeharsha Abdulrahman Ibrahim Altaysan Abdulmalek Ahmed Balgoname |
| author_sort | Mahesh Attimarad |
| collection | DOAJ |
| description | A combination of antibiotics and antiprotozoal and antisecretory medicines has been prescribed for the treatment of diarrhea. A rapid, reproducible liquid chromatographic procedure was established for the concurrent analysis of metronidazole (MET), ofloxacin (OFL), and racecadotril (RAC) in suspension. The Box–Behnken design, a full factorial multivariate optimization technique, was utilized to optimize chromatographic parameters with fewer runs. The separation of MET, OFL, and RAC was accomplished within 3.2 min, using a Zorbax C<sub>18</sub> high-performance liquid chromatography column with a simple mobile phase comprising acetonitrile (55 vol.%): methanol (10 vol.%):20 mM phosphate buffer (35 vol.%, pH 6, regulated with ortho-phosphoric acid). The mobile phase was pumped in the isocratic mode at a rate of 1.4 mL/min at ambient temperature. Analytes were monitored by adjusting the wavelength at 295 nm for MET and OFL and 231 nm for RAC. Validation of the proposed HPLC method exhibited linearity in the concentration of 20–250 µg/mL, 10–150 µg/mL, and 5–80 µg/mL for MET, OFL, and RAC respectively, along with an excellent regression coefficient (r<sup>2</sup> > 0.999). The accuracy and precision of the chromatographic procedure were also evidenced by the low percent relative error and relative standard deviation. A Pareto chart developed by the two-factor interaction (2FI) study confirmed that the method was robust, as the slight variation in a single factor had no significant influence on the assay outcomes. Lastly, the developed HPLC process was utilized for the concurrent quantification of MET, OFL, and RAC in liquid oral preparation. Furthermore, when the assay results were compared to the described techniques, it was discovered that there was no significant difference in the accuracy and precision of the results. Hence, the developed rapid HPLC method could be employed for the quality control study of a preparation comprising of MET, OFL, and RAC in industries and regulatory authority laboratories. |
| first_indexed | 2024-03-10T01:51:58Z |
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| id | doaj.art-6e21e7e3056e4d10aa021b3aa2ecf019 |
| institution | Directory Open Access Journal |
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| language | English |
| last_indexed | 2024-03-10T01:51:58Z |
| publishDate | 2022-04-01 |
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| spelling | doaj.art-6e21e7e3056e4d10aa021b3aa2ecf0192023-11-23T13:04:17ZengMDPI AGSeparations2297-87392022-04-019510310.3390/separations9050103Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response MethodologyMahesh Attimarad0Katharigatta Narayanaswamy Venugopala1Muhammad S. Chohan2Pottathil Shinu3Marysheela David4Effren II Plaza Molina5Anroop Balachandran Nair6Nagaraja Sreeharsha7Abdulrahman Ibrahim Altaysan8Abdulmalek Ahmed Balgoname9Department of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Biomedical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Biomedical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Nursing, College of Applied Medical Sciences, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmacy Practice, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaDepartment of Pharmaceutical Sciences, College of Clinical Pharmacy, King Faisal University, Al-Ahsa 31982, Saudi ArabiaA combination of antibiotics and antiprotozoal and antisecretory medicines has been prescribed for the treatment of diarrhea. A rapid, reproducible liquid chromatographic procedure was established for the concurrent analysis of metronidazole (MET), ofloxacin (OFL), and racecadotril (RAC) in suspension. The Box–Behnken design, a full factorial multivariate optimization technique, was utilized to optimize chromatographic parameters with fewer runs. The separation of MET, OFL, and RAC was accomplished within 3.2 min, using a Zorbax C<sub>18</sub> high-performance liquid chromatography column with a simple mobile phase comprising acetonitrile (55 vol.%): methanol (10 vol.%):20 mM phosphate buffer (35 vol.%, pH 6, regulated with ortho-phosphoric acid). The mobile phase was pumped in the isocratic mode at a rate of 1.4 mL/min at ambient temperature. Analytes were monitored by adjusting the wavelength at 295 nm for MET and OFL and 231 nm for RAC. Validation of the proposed HPLC method exhibited linearity in the concentration of 20–250 µg/mL, 10–150 µg/mL, and 5–80 µg/mL for MET, OFL, and RAC respectively, along with an excellent regression coefficient (r<sup>2</sup> > 0.999). The accuracy and precision of the chromatographic procedure were also evidenced by the low percent relative error and relative standard deviation. A Pareto chart developed by the two-factor interaction (2FI) study confirmed that the method was robust, as the slight variation in a single factor had no significant influence on the assay outcomes. Lastly, the developed HPLC process was utilized for the concurrent quantification of MET, OFL, and RAC in liquid oral preparation. Furthermore, when the assay results were compared to the described techniques, it was discovered that there was no significant difference in the accuracy and precision of the results. Hence, the developed rapid HPLC method could be employed for the quality control study of a preparation comprising of MET, OFL, and RAC in industries and regulatory authority laboratories.https://www.mdpi.com/2297-8739/9/5/103HPLCsurface responsemultivariate optimizationformulationmetronidazoleofloxacin |
| spellingShingle | Mahesh Attimarad Katharigatta Narayanaswamy Venugopala Muhammad S. Chohan Pottathil Shinu Marysheela David Effren II Plaza Molina Anroop Balachandran Nair Nagaraja Sreeharsha Abdulrahman Ibrahim Altaysan Abdulmalek Ahmed Balgoname Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology Separations HPLC surface response multivariate optimization formulation metronidazole ofloxacin |
| title | Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology |
| title_full | Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology |
| title_fullStr | Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology |
| title_full_unstemmed | Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology |
| title_short | Multivariate Optimization of Chromatographic Conditions for Rapid Simultaneous Quantification of Antidiarrheal Drugs in Formulation Using Surface Response Methodology |
| title_sort | multivariate optimization of chromatographic conditions for rapid simultaneous quantification of antidiarrheal drugs in formulation using surface response methodology |
| topic | HPLC surface response multivariate optimization formulation metronidazole ofloxacin |
| url | https://www.mdpi.com/2297-8739/9/5/103 |
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