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DEVELOPMENT OF A PRECOLUMN DERIVATIZATION METHOD FOR THE QUANTITATIVE DETECTION OF ETHYLENEDIAMINE IMPURITY IN PHARMACEUTICAL DRUGS USING RP-HPLC COUPLED WITH UV/PDA DETECTOR

By: Contributor(s): Description: Page No. 44-51Subject(s): In: Indian Drugs Mumbai Indian Drugs Manufacturer's AssociationSummary: The proposed study aimed to create and validate a technique for detecting impurities in drug substances, specifically targeting low levels of ethylenediamine in pharmaceutical raw materials. The method involved the use of benzoyl chloride as a derivatizing agent, during pre-column derivatization processing, effectively boosting the sensitivity and precision of the method. Chromatographic conditions were optimized, including the use of 0.7g L-1 di-sodium hydrogen phosphate anhydrous and methanol, a specific XBridgeTM Shield RP-18 column, 10μL injection volume, and a flow rate of 0.8mL min-1 at 25°C. This method combined precolumn derivatization with RP-HPLC UV/PDA detection, proving highly sensitive and precise with favorable linearity (r ≥ 0.99) and precision (% RSD/CV < 5.0) upon validation. The developed method is noted for its simplicity, speed, cost-effectiveness, and suitability for regular analysis in QC labs, particularly for detecting impurities in drug candidates.
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Item type Current library Call number Vol info Status Barcode
Journal Article SNDT Juhu Available jp940.4
Periodicals SNDT Juhu P 615.8805/ID (Browse shelf(Opens below)) Vol. 62, No. 3 (01/03/2025) Available JP940

The proposed study aimed to create and validate a technique for detecting impurities in drug substances, specifically targeting low levels of ethylenediamine in pharmaceutical raw materials. The method involved the use of benzoyl chloride as a derivatizing agent, during pre-column derivatization processing, effectively boosting the sensitivity and precision of the method. Chromatographic conditions were optimized, including the use of 0.7g L-1 di-sodium hydrogen phosphate anhydrous and methanol, a specific XBridgeTM Shield RP-18 column, 10μL injection volume, and a flow rate of 0.8mL min-1 at 25°C. This method combined precolumn derivatization with RP-HPLC UV/PDA detection, proving highly sensitive and precise with favorable linearity (r ≥ 0.99) and precision (% RSD/CV < 5.0) upon validation. The developed method is noted for its simplicity, speed, cost-effectiveness, and suitability for regular analysis in QC labs, particularly for detecting impurities in drug candidates.

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