Chromatography Forum

Hi everybody,
we have to develope a method for the analysis of impurities in a pharmaceutical product. We have to use HPLC-UV for the quantification of the impurities.
The product is a softgel capsule containing the active ingredient (low concentration) and some excipients. When we dissolve the capsule (2 cps in 10mL of 50%MeOH in water) we obtain a gelatinous liquid.
The main excipients are hard-soft gelatin and glicerin.
There is a way to selectively remove this excipients from the active ingredient?
What is the normal sample preparation for softgel campsules (just dissolution, filtration and injection) or there is something else (SPE, etc)?

Any suggestions?

Have a good day,

Davide

Admittedly its been a while since I've done any soft-gel analytical work.

I don't think we did anything out of the ordinary with it (just dissolution with aq. AcN) and then syringe filtered samples.

If you have access to placebo formulations ensure you don't get any interfering peaks from this.

I have developed a method for the separation of gelatine and low molecular components using coupled columns.

Principle:
Dissolve entire sample
Inject on a size-exclusion column
After elution of gelatine, collect the peaks on a precolumn
elute the precolumn to an analytical column and detect your peaks without interferences.

I works super-fine for my applicatuion and everything is automated (so you can go home and see the World Cup)

If you are interested I can send you a copy of the poster presentation from HPLC2005.

To Mattias: I'd love a copy of your HPLC 2005 poster on gelatin capsules. Please send to tleusner@cephalon.com.

Question: Has anyone had Tween 80 in their soft gels or liquid formulas? If so, does your column eventually get affected by the Tween 80 and/or how do you handle the situation.

To Mattias: I'd love a copy of your HPLC 2005 poster on gelatin capsules. Please send to : ramiaqu@batelco.jo