QUANTIFICATION OF HAZARDOUS HIGH BOILING SOLVENTS IMPURITIES IN ANTI-DIABETIC DRUG LINAGLIPTIN BY NOVEL GC-ALS METHOD DEVELOPMENT AND VALIDATION

Abstract

A new precise and accurate GC-ALS method was developed and validated for quantitative determination of hazardous high boiling solvents impurities i.e. acetic acid and dimethyl sulphoxide in Linagliptin drug molecule using direct injection technique by GC-ALS with the help of Flame ionization detector (FID). The column used was Agilent J & W DB-FFAP, 30M X 0.530 mm X 1µm capillary column. The stationary phase of the column was nitro terephthalic acid-modified polyethylene glycol (PEG). The method was validated for specificity, precision, LOD, LOQ, accuracy, linearity, range, solution stability, and robustness. The detection limit and quantitation limit obtained for acetic acid was 83.3µg/g and 252.4 µg/g respectively. For Dimethyl sulphoxide detection limit and quantitation limit obtained were 83.7 µg/g and 253.7 µg/g respectively. The method was found to be linear in the range between 253.9 µg/g to 7616.9 µg/g for acetic acid and 253.5 µg/g to 7605.8 µg/g for dimethyl sulphoxide. The average recoveries obtained were 85.20% and 89.69% at LOQ level for acetic acid and dimethyl sulphoxide respectively, and for 150% level recovery were 94.26% and 100.43% for acetic acid and dimethyl sulphoxide respectively. The developed method was found to be robust, specificity was also demonstrated, and standard and the spiked solution was stable for up 20 Hrs. Thus, the method is used for routine analysis of their intended use. For quantification of Acetic acid and Dimethyl sulphoxide in Linagliptin, no pharmacopeial method is available so developed this simple method for laboratory use.