-
- Posts: 20
- Joined: Tue Aug 10, 2010 5:39 pm
- Location: india
We are developing method for analysis of 3-chloropropylaine HCl content in one of our intermediates. As the compound is non-UV active, the method is developed on HPLC-RI.
MP: 0.1% HFBA in water.
Column: C18, 250 mm x 4.6 mm, 5 micron
Diluent: Mobile phase
Whenever I inject 3-chloropropylamine HCl standard, I always observe two peaks, one eluting very early (about 2 min) and one eluting later (about 13 minutes). Initially, we thought that the early eluting peak belongs to HCl salt. Accordingly, we injected HCl (since the impurity contains about 28% HCl by weight, for 100 ppm of impurity, we checked the retention time of HCL at 28 ppm level) but found an almost negligible peak eluting at the retention time of early eluting peak, much smaller than that observed in 3-chloropropylamine HCl. We also tried to break the salt, isolating the impurity and injecting it. However, we still observed the peak but smaller than that observed in salt.
In salt the peak ratio was 28:72
In base the peak ratio was 7:92.
Shall we consider this peak as belonging to HCl or any other reaction is happening within the solution (we tried different diluents but the pattern remains same). Please suggest.
Best regards,
Andy