Abstract
Three known and one unknown impurities in salbutamol sulphate bulk drug at level 0.1% (ranging from 0.05-0.1%) were detected by gradient reverse phase high performance liquid chromatography. These impurities were preliminarily identified by the mass number of the impurities. Different experiments were conducted and finally synthesized and characterized the known and unknown imputities.
Highlights
Salbutamol sulphate is a relatively selective 2-adrenergic agonist and is used as a bronchodilator
Sample was analyzed by High performance liquid chromatography (HPLC) and its purity was found to be 93.14%, molecular weight of salbutamol sulphate impurity-1 is 253.34 which is 14 mass unit higher than that of salbutamol sulphate
The ESI mass spectrum of sample gave a protonated molecular ion at m/z 254.1 and deprotonated molecular ion at m/z 252.6 which is the same as salbutamol sulphate impurity-127-30, IR spectrum displayed characteristic absorptions at 3398.89 & 2982.02,2934.06 cm-1 corresponding to >NH and aromatic >CH stretching .The peaks at 1509.95 & 1452.92 cm-1 in IR spectrum is indicative of >C=C< ring stretching, the chemical shift of the 1H signals showed an additional signal at 3.15 ppm as singlet, which could be attributed to a methoxy group present in impurity-1, 13C signals showed an additional signal at 49.84 ppm, which could be attributed to a methoxy group present in impurity-1
Summary
Salbutamol sulphate is a relatively selective 2-adrenergic agonist and is used as a bronchodilator. A literature search revealed that only analytical procedure[7,8,9] is available but nobody has reported synthesis, isolation and characterization of impurities in the purified form starting from salbutamol sulphate. Isolation and Characterization of Process-Related Impurities 1722 shift values were reported relative to CDCl3 (δ=77.00 ppm) and DMSO, d6 (δ=39.50 ppm)as internal standards. Salbutamol base 2 g was charged with 50 mL acetone into one neck round bottom flask with magnatic stirrer K2CO3 (1.2 g) was added and heating started with stirring. To this benzylchloride 1.1 g was added and contents refluxed for 12 h. This peak was purified using preparative HPLC and marked as fraction-4 (Scheme 2)
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