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Method Development and Validation of Ion Chromatography Method for Determination of Free Sulfate in Fondaparinux Sodium Pre-Filled Syringe
Corresponding Author(s) : Narasimha S. Lakka
Asian Journal of Chemistry,
Vol. 32 No. 7 (2020): Vol 32 Issue 7
Abstract
A simple ion chromatography method was developed for the quantitative determination of free sulfate in fondaparinux sodium pre-filled syringe for injection. Chromatographic separation was achieved on an anion-exchange resin column made of super macro porous polyvinyl benzyl ammonium polymer cross-linked with divinyl benzene (250 × 4.0 mm) with a mobile phase consisting of 60 mM carbonate buffer solution. Conductivity detector was employed with a flow rate of 0.7 mL min-1, injection volume of 100 μL and column temperature of 30 ºC. Retention time of sulfate (SO42−) was eluted at about 10.4 min. The developed method was validated in according to ICH Q2(R1) guideline and was found to be specific, precise, accurate, linear and robust. The precision was evaluated with six individual spiked samples of sulfate on Fondaparinux sodium for injection. The proposed method is linear (r2 > 0.9991) and accurate, mean recoveries were 99.2-117.8 % at 3 different levels (50-150%). The robustness was performed by changing the flow rate of mobile phase (0.7 ± 0.1 mL min-1) and column temperature (30 ± 2 ºC). The proposed method is capable to determine free sulphate in fondaparinux sodium for injection in presence of excipients used in pharmaceutical formulation and also in its active pharmaceutical ingredient.
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- ARIXTRA® (fondaparinux sodium) Injection; Accessed on October 05, 2019. https://www.accessdata.fda.gov/drugsatfda_docs/label/2005/021345s010lbl.pdf.
- Sulfate in Drinking-Water, Background Document for Development of WHO Guidelines for Drinking-Water Quality, WHO/SDE/WSH/03.04/114. Accessed on October 05, 2019.
- R. Michalski, Crit. Rev. Anal. Chem., 39, 230 (2009); https://doi.org/10.1080/10408340903032453
- Y.M. Moustafa and R.E. Morsi, Ion Exchange Chromatography-An Overview, InTech Open (2013);
- Fondaparinux Sodium, USP Monograph, USP 40, pp 4324-4327 (1982).
- Fondaparinux Sodium Injection, USP Monograph, USP 40, pp 4327-4329 (1982).
- The United States Pharmacopeia, Validation of Compendial Methods, USP 41-NF 36, Chap. 1225 (2018).
- ICH Guideline, Q2(R1) Validation of Analytical Procedure: Text and Methodology (2005).
References
ARIXTRA® (fondaparinux sodium) Injection; Accessed on October 05, 2019. https://www.accessdata.fda.gov/drugsatfda_docs/label/2005/021345s010lbl.pdf.
Sulfate in Drinking-Water, Background Document for Development of WHO Guidelines for Drinking-Water Quality, WHO/SDE/WSH/03.04/114. Accessed on October 05, 2019.
R. Michalski, Crit. Rev. Anal. Chem., 39, 230 (2009); https://doi.org/10.1080/10408340903032453
Y.M. Moustafa and R.E. Morsi, Ion Exchange Chromatography-An Overview, InTech Open (2013);
Fondaparinux Sodium, USP Monograph, USP 40, pp 4324-4327 (1982).
Fondaparinux Sodium Injection, USP Monograph, USP 40, pp 4327-4329 (1982).
The United States Pharmacopeia, Validation of Compendial Methods, USP 41-NF 36, Chap. 1225 (2018).
ICH Guideline, Q2(R1) Validation of Analytical Procedure: Text and Methodology (2005).