Cost Effective Quantification of Trace Level edta (Ethylene Di-amine Tetra Acetic Acid) by Titrimetry in Active Pharmaceutical Ingredients

Method parameters: Instrument parameters
Method validation
Method 
Validation [7,8] 
is the process used to confirm that the analytical procedure employed for a specific test is 
suitable for its intended use. Results from method validation can be used to judge the quality, reliability and consistency 

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Nagaraju et al
Der Chemica Sinica, 2017, 8(1):175-183
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of analytical results; it is an integral part of any good analytical practice.
The potentiometric titration method was developed and validated according to International Conference on 
Harmonization (ICH) guidelines for validation of analytical procedures [9]. The method was validated for the 
parameters like Linearity, accuracy, system precision, Intra-day precision, Inter-day precision, intermediate precision/
Ruggedness, Robustness, Limit of detection (LOD) and Limit of quantitation (LOQ).
Specificity
Specificity is the ability of the method to measure the analyte response in the presence of all impurities related 
to drug substance, for specificity determination checking the interference of Blank, EDTA [9-11] spiked to drug 
substance at known concentration level and all known related substances of drug substance including EDTA [12-14] 
with known concentration level were prepared and analysed and Perform the EDTA Content the percentage difference 
between EDTA content in spiked individually and spiked with known related substance was determined. Calculate the 
percentage difference between spiked and unspiked.
Linearity
Standard solutions of EDTA at different concentrations were prepared. Calibration curve was performed by plotting 
the concentration level of EDTA (Ethylene di amine tetra acetic acid) versus corresponding volume of 0.01 M Copper 
sulphate consumed in the titration. Accurately weighed 1.5211 g of EDTA.2Na (Which is equivalent to EDTA) in a 
250 ml volumetric flask sonicate to dissolve and make up to the mark with water. To this take separately with micro 
pipette 100 µl, 150 µl, 200 µl, 250 µl, 300 µl to all the solutions add 10 ml of PH:10 buffer add 60 ml water swirl well 
to dissolve then titrate with 0.01 M Copper sulphate solution determine the end point potentiometrically note down the 
volume as V1 (ml). Calibration curve was constructed by plotting the concentration of EDTA (in mg) versus volume 
of 0.01 M Copper sulphate solution. The result show an excellent correlation between volume of copper sulphate 
consumed and concentration of EDTA with in the concentration range (w.r.t sample concentration 0.05% to 0.15%) 
are given. The correlation coefficient was greater than 0.999, which meet the method validation acceptance criteria 
and hence the method is said to be linear (Table 1).