Gummi Base Troche Extraction

Discussions about sample preparation: extraction, cleanup, derivatization, etc.

8 posts Page 1 of 1
We've been using the USP Monograph for Progesterone Compounded Vaginal Inserts to test our Progesterone creams, tablets/capsules, and troches for potency. However, everything but the gummi base troches have passed within the necessary acceptance criteria.
In short, we dissolved one troche in 200mL of progesterone mobile phase (55 reagent alcohol to 45 water), sonicated before filling to volume, and performing filtration (only using the last 6mL of total 10mL filtered) and dilution when needed. We're using a Waters C18 Nova-Pak 3.9x15mm 4mcm particle size and ran our samples at 245nm - RP-HPLC-PDA but no QDa used yet.
Our average percent yield over the course of a week of testing is 66%.
So I tried making the mobile phase 50:50 and ran the samples at 245nm and 254nm. The calibration curve for each method (A,B,C) was r^2 = 0.9995 each time on average.
We're also going to switch from distilled water to LC-MS grade water and have ordered new guard columns...potentially the last samples in the past could have clogged the column or dirtied it before I even started working here?
We also found this paper https://www.ncbi.nlm.nih.gov/pubmed/15595573 that says to actually melt the suppository (they use a dosage form that has a similar matrix to our troches) before dissolving it. Do you think melting will release that progesterone from the matrix?
Looking for other ideas as to why we're not seeing 90-110% yield of progesterone from compounded glycerin-gelatin-water troches...
I am going to think gelatin will prevent the extraction of progesterone. However, there is an easy solution! Just take a troche and add 50 ml of hot water (gelatin is dissolved by hot water). Swirl and sonicate the solution. Bring it up to 100 mL with mobile phase, shake it, syringe filter a portion and inject.
So the hot water will be different from the room temperature water in the mobile phase that is heated to 40C on a hot plate?

Thanks!
Yep. 40C, mix, spin down and/or filter and shoot.
Thanks,
DR
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I've been experiencing the same issue with the Testosterone gummi base troches so I'll try this on both!

Thanks!
I was trying to do Vitamin Bs from a gummi vitamin in the past and it was nearly impossible to dissolve the gummi. I finally figured out that if I just put it in water then placed it in a microwave for abotu 30-60seconds the gummi would dissolve and release the vitamins. If you have the gummi that is made from a mixture of gelatin and bee's wax it just doesn't dissolve well in either organic or aqueous solution, but the microwave will cause the wax to melt and it will dissolve easily then.
The past is there to guide us into the future, not to dwell in.
Do you think that would work on a troche made of gelatin, glycerin, and water? I don't know if the glycerin in our troches would behave similar to the bees wax in yours. I'm considering melting it in a water bath...
It might work. Pop it in a microwave in a beaker with about 50-100ml water and just watch it for a minute. The gummi vitamin I was working with just fell apart after about 45 seconds.
The past is there to guide us into the future, not to dwell in.
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