Research Article

Stability-Indicating Gradient RP-LC Method for the Determination of Process and Degradation Impurities in Bosentan Monohydrate: An Endothelin Receptor Antagonist

Table 1

Mass, FTIR spectral data and 1H NMR chemical shift values.

Name of ImpurityMass value (m/z) (M+H)+FT-IR (KBr) absorption bands (cm−1)1H NMR Chemical shift values, δ in ppm, (multiplicity, integration)

(1) Imp-A526.013379.95, 3053.28, 2960.51, 2866.72, 2903.48, 2960.51, 1248.99, 1347.78, 1176.07, 1663.97, 1080.95, 1551.24, 719.428.76-8.77 (d, 2H), 7.45 (t, 1H), 6.86–6.94 (d, 3H), 6.67–6.71 (t, 1H), 6.48–6.50 (t, 1H), 7.48 (s, 1H), 7.09–7.11 (d, 3H), 1.2 (s, 9H), 3.75 (s, 3H)
(2) Imp-B508.493447.92, 3214.78, 3039.63, 2962.43, 2869.34, 2962.43, 1248.00, 1345.77, 1170.86, 1663.72, 1081.03, 1565.46, 759.238.99–9.02 (d, 2H), 7.45–7.55 (t, 1H), 11.1 (s, 1H), 6.95–7.03 (d, 1H), 7.07–7.14 (t, 1H), 6.84–6.94 (t, 1H), 9.1 (s, 1H), 8.35–8.45 (d, 2H), 7.40–7.44 (d, 3H), 1.3 (s, 9H), 6.84–6.94 (s, 3H)
(3) Imp-C1041.203063.53, 2963.28, 2837.57, 2869.63, 1574.76, 1558.52, 1335.83, 1257.85, 1257.07, 1163.09, 749.828.98 (d, 4H, CH), 8.89 (t, 2H), 4.00 (t, 2H), 3.81 (t, 2H), 6.13-6.99 (m, 8H), 8.29 (s, 2H), 3.72 (s, 6H), 7.25–7.32 (d, 4H), 7.44 (d, 4H), 1.09–1.17 (s, 18H)
(4) Imp-D350.843068.47, 2839.99, 1603.24, 1587.66, 1456.61, 1134.38, 752.099.04–9.06 (d, 2H), 7.46–7.49 (t, 1H), 6.78–6.80 (d, 1H), 6.88–6.93 (t, 1H), 7.11–7.16 (t, 1H), 6.99–7.02 (d, 1H), 3.86 (s, 3H)
(4) Imp-E214.501328.75, 1165.96, 1268.00, 1568.44, 832.37, 3268.89, 2963.78, 3363.817.50–7.53 (d, 2H), 7.82–7.85 (d, 2H), 1.33 (s, 9H), 4.83 (s, 2H)

S: singlet; m: multiplet; t: triplet; d: doublet.