In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis
Autori
Osmanović Omerdić, EhlimanaAlagić-Džambić, Larisa
Krstić, Marko
Pašić-Kulenović, Maja
Odović, Jadranka
Vasiljević, Dragana
Članak u časopisu (Objavljena verzija)
Metapodaci
Prikaz svih podataka o dokumentuApstrakt
Solid dispersions were prepared via a solvent evaporation method, employing ethanol (96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer 407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for the simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release from solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of acetonitrile-methanol-phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min. The method was validated according to International Conference of Harmonisation guidelines and validation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD), and limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and clopidogrel bisulfate. The linearity was provided in the concentration range 0.0275-0.1375 mg/mL for acetylsalicylic acid and 0.020...0-0.1000 mg/mL for clopidogrel bisulfate, with a correlation coefficient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was confirmed by calculated recoveries for acetylsalicylic acid (98.6-101.0%) and clopidogrel bisulfate (100.0-101.6%). The intra-day and the inter-day precision-calculated relative standard deviations are less than 1%, which indicates high precision of the method. The limits of detection and quantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate 0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did not significantly affect qualitative and quantitative system responses, which proved robustness of method. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel bisulfate and acetylsalicylic acid from solid dispersions.
Ključne reči:
Acetylsalicylic acid / Clopidogrel bisulfate / Dissolution / RP-HPLC / Solid dispersion / ValidationIzvor:
Applied Sciences (Switzerland), 2020, 10, 14Izdavač:
- MDPI AG
DOI: 10.3390/app10144792
ISSN: 2076-3417
WoS: 000554858500001
Scopus: 2-s2.0-85088659853
Institucija/grupa
PharmacyTY - JOUR AU - Osmanović Omerdić, Ehlimana AU - Alagić-Džambić, Larisa AU - Krstić, Marko AU - Pašić-Kulenović, Maja AU - Odović, Jadranka AU - Vasiljević, Dragana PY - 2020 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3637 AB - Solid dispersions were prepared via a solvent evaporation method, employing ethanol (96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer 407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for the simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release from solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of acetonitrile-methanol-phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min. The method was validated according to International Conference of Harmonisation guidelines and validation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD), and limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and clopidogrel bisulfate. The linearity was provided in the concentration range 0.0275-0.1375 mg/mL for acetylsalicylic acid and 0.0200-0.1000 mg/mL for clopidogrel bisulfate, with a correlation coefficient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was confirmed by calculated recoveries for acetylsalicylic acid (98.6-101.0%) and clopidogrel bisulfate (100.0-101.6%). The intra-day and the inter-day precision-calculated relative standard deviations are less than 1%, which indicates high precision of the method. The limits of detection and quantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate 0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did not significantly affect qualitative and quantitative system responses, which proved robustness of method. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel bisulfate and acetylsalicylic acid from solid dispersions. PB - MDPI AG T2 - Applied Sciences (Switzerland) T1 - In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis VL - 10 IS - 14 DO - 10.3390/app10144792 ER -
@article{ author = "Osmanović Omerdić, Ehlimana and Alagić-Džambić, Larisa and Krstić, Marko and Pašić-Kulenović, Maja and Odović, Jadranka and Vasiljević, Dragana", year = "2020", abstract = "Solid dispersions were prepared via a solvent evaporation method, employing ethanol (96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer 407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for the simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release from solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of acetonitrile-methanol-phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min. The method was validated according to International Conference of Harmonisation guidelines and validation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD), and limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and clopidogrel bisulfate. The linearity was provided in the concentration range 0.0275-0.1375 mg/mL for acetylsalicylic acid and 0.0200-0.1000 mg/mL for clopidogrel bisulfate, with a correlation coefficient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was confirmed by calculated recoveries for acetylsalicylic acid (98.6-101.0%) and clopidogrel bisulfate (100.0-101.6%). The intra-day and the inter-day precision-calculated relative standard deviations are less than 1%, which indicates high precision of the method. The limits of detection and quantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate 0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did not significantly affect qualitative and quantitative system responses, which proved robustness of method. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel bisulfate and acetylsalicylic acid from solid dispersions.", publisher = "MDPI AG", journal = "Applied Sciences (Switzerland)", title = "In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis", volume = "10", number = "14", doi = "10.3390/app10144792" }
Osmanović Omerdić, E., Alagić-Džambić, L., Krstić, M., Pašić-Kulenović, M., Odović, J.,& Vasiljević, D.. (2020). In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis. in Applied Sciences (Switzerland) MDPI AG., 10(14). https://doi.org/10.3390/app10144792
Osmanović Omerdić E, Alagić-Džambić L, Krstić M, Pašić-Kulenović M, Odović J, Vasiljević D. In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis. in Applied Sciences (Switzerland). 2020;10(14). doi:10.3390/app10144792 .
Osmanović Omerdić, Ehlimana, Alagić-Džambić, Larisa, Krstić, Marko, Pašić-Kulenović, Maja, Odović, Jadranka, Vasiljević, Dragana, "In vitro dissolution study of acetylsalicylic acid and clopidogrel bisulfate solid dispersions: Validation of the RP-HPLC method for simultaneous analysis" in Applied Sciences (Switzerland), 10, no. 14 (2020), https://doi.org/10.3390/app10144792 . .