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Scientia Pharmaceutica is published by MDPI from Volume 84 Issue 3 (2016). Previous articles were published by another publisher in Open Access under a CC-BY (or CC-BY-NC-ND) licence, and they are hosted by MDPI on mdpi.com as a courtesy and upon agreement with Austrian Pharmaceutical Society (Österreichische Pharmazeutische Gesellschaft, ÖPhG).
Article

Novel, Precise, Accurate Ion-Pairing Method to Determine the Related Substances of the Fondaparinux Sodium Drug Substance: Low-Molecular-Weight Heparin

1
Analytical Research, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories Ltd., Bollaram road, Miyapur, Hyderabad-500049 (AP), India.
2
Department of Physical, Nuclear and Chemical Oceanology, Andhra University, Visakhapatnam-530003, India.
*
Author to whom correspondence should be addressed.
Sci. Pharm. 2016, 84(1), 19-40; https://doi.org/10.3797/scipharm.1505-20
Received: 26 May 2015 / Accepted: 22 July 2015 / Published: 22 July 2015
Fondaparinux sodium is a synthetic low-molecular-weight heparin (LMWH). This medication is an anticoagulant or a blood thinner, prescribed for the treatment of pulmonary embolism and prevention and treatment of deep vein thrombosis. Its determination in the presence of related impurities was studied and validated by a novel ion-pair HPLC method. The separation of the drug and its degradation products was achieved with the polymer-based PLRPs column (250 mm × 4.6 mm; 5 μm) in gradient elution mode. The mixture of 100 mM n-hexylamine and 100 mM acetic acid in water was used as buffer solution. Mobile phase A and mobile phase B were prepared by mixing the buffer and acetonitrile in the ratio of 90:10 (v/v) and 20:80 (v/v), respectively. Mobile phases were delivered in isocratic mode (2% B for 0–5 min) followed by gradient mode (2–85% B in 5–60 min). An Evaporative Light Scattering Detector (ELSD) was connected to the LC system to detect the responses of chromatographic separation. Further, the drug was subjected to stress studies for acidic, basic, oxidative, photolytic, and thermal degradations as per ICH guidelines and the drug was found to be labile in acid, base hydrolysis, and oxidation, while stable in neutral, thermal, and photolytic degradation conditions. The method provided linear responses over the concentration range of the LOQ to 0.30% for each impurity with respect to the analyte concentration of 12.5 mg/mL, and regression analysis showed a correlation coefficient value (r2) of more than 0.99 for all the impurities. The LOD and LOQ were found to be 1.4 μg/mL and 4.1 μg/mL, respectively, for fondaparinux. The developed ion-pair method was validated as per ICH guidelines with respect to accuracy, selectivity, precision, linearity, and robustness
Keywords: Fondaparinux sodium; HPLC-ELSD; Validation; Purity; Related Substance; Ion pair Fondaparinux sodium; HPLC-ELSD; Validation; Purity; Related Substance; Ion pair
MDPI and ACS Style

DESHPANDE, A.A.; MADHAVAN, P.; DESHPANDE, G.R.; CHANDEL, R.K.; YARBAGI, K.M.; JOSHI, A.R.; BABU, J.M.; MURALI KRISHNA, R.; RAO, I.M. Novel, Precise, Accurate Ion-Pairing Method to Determine the Related Substances of the Fondaparinux Sodium Drug Substance: Low-Molecular-Weight Heparin. Sci. Pharm. 2016, 84, 19-40. https://doi.org/10.3797/scipharm.1505-20

AMA Style

DESHPANDE AA, MADHAVAN P, DESHPANDE GR, CHANDEL RK, YARBAGI KM, JOSHI AR, BABU JM, MURALI KRISHNA R, RAO IM. Novel, Precise, Accurate Ion-Pairing Method to Determine the Related Substances of the Fondaparinux Sodium Drug Substance: Low-Molecular-Weight Heparin. Scientia Pharmaceutica. 2016; 84(1):19-40. https://doi.org/10.3797/scipharm.1505-20

Chicago/Turabian Style

DESHPANDE, Amol A., P. MADHAVAN, Girish R. DESHPANDE, Ravi K. CHANDEL, Kaviraj M. YARBAGI, Alok R. JOSHI, J. M. BABU, R. MURALI KRISHNA, and I. M. RAO 2016. "Novel, Precise, Accurate Ion-Pairing Method to Determine the Related Substances of the Fondaparinux Sodium Drug Substance: Low-Molecular-Weight Heparin" Scientia Pharmaceutica 84, no. 1: 19-40. https://doi.org/10.3797/scipharm.1505-20

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