Trace Determination of Azodiisobutyronitrile in Rupatadine Fumarate by GC-MS

OBJECTIVE To establish a GC-MS analytical method for the trace determination of azodiisobutyronitrile (AIBN) in Rupatadine Fumarate. METHODS The analytical column was DB-624(30 m×0.25 mm, 1.4 μm). The column temperature was maintained at 70℃, then was raised to 250℃ at the rate of 12℃·min^-1, and the flow rate was 0.6 mL·min^-1, the conditions of GC-MS were optimized. The detection was achieved in EI, and the selected ions were m/z 69, m/z 54 and m/z 41. RESULTS The calibration curve of AIBN was in a good linearity over the range of 0.155 2-3.103 μg·mL^-1(r²=0.999 8). The limit of detection was 0.045 μg·mL^-1, and the limit of quantification was 0.15 μg·mL^-1. Repetition of AIBN was fine, with RSD(n=6) of 0.31%. The recoveries of low, middle and high adding concentrations of AIBN were 103.9%, 101.0% and 99.4%, respectively, and the RSD(n=3) were 0.03%, 0.11% and 0.08%. AIBN was not detected in 3 batches of samples. CONCLUSION The method has been proved to be simple, rapid and reliable, which is applicable for the quality control of AIBN in Rupatadine Fumarate.