Open AccessMethod Development and Validation of Ion Chromatography Method for Determination of Free Sulfate in Fondaparinux Sodium Pre-Filled Syringe
Author(s) -
Kona S Srinivas,
Mahesh Kalva,
Mallesh Changali,
Narasimha S. L akka
Publication year - 2020
Publication title -
asian journal of chemistry/asian journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.145
H-Index - 34
eISSN - 0975-427X
pISSN - 0970-7077
DOI - 10.14233/ajchem.2020.22674
Subject(s) - chemistry , chromatography , syringe driver , elution , sodium sulfate , syringe , volumetric flow rate , ion chromatography , sodium , psychology , physics , organic chemistry , quantum mechanics , psychiatry
A simple ion chromatography method was developed for the quantitative determination of free sulfatein fondaparinux sodium pre-filled syringe for injection. Chromatographic separation was achieved onan anion-exchange resin column made of super macro porous polyvinyl benzyl ammonium polymercross-linked with divinyl benzene (250 × 4.0 mm) with a mobile phase consisting of 60 mM carbonatebuffer solution. Conductivity detector was employed with a flow rate of 0.7 mL min-1, injection volumeof 100 μL and column temperature of 30 ºC. Retention time of sulfate (SO42−) was eluted at about 10.4min. The developed method was validated in according to ICH Q2(R1) guideline and was found to bespecific, precise, accurate, linear and robust. The precision was evaluated with six individual spikedsamples 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 wasperformed by changing the flow rate of mobile phase (0.7 ± 0.1mL min-1) and column temperature (30± 2 ºC). The proposed method is capable to determine free sulphate in fondaparinux sodium forinjection in presence of excipients used in pharmaceutical formulation and also in its activepharmaceutical ingredient.