I have used two polymer called PCL and PLGA in 50:50 ratio to make electrospun nanofiber. Are they going be present still in 50:50 ratio in the nanofiber? Is it possible to determine by NMR?
Dear Jakia Khanom, first you should decide on the type of NMR to be used, there a broad informative differences between solid and solution states NMR tools. Solid state NMR is more suited since it reflects the actual phase repartion of the polymers forming the blend. Please have a look at the following documents. My Regards
Yes, this is possible using 1H NMR. You should be able to determine the lactic, glycolic and caprolactam content of the polymer mixture, as characterictic signals of each monomer can be found in the NMR spectrum.
I'd be hesitative to say yes (in liquid state) out of the following reason:
I do not know how you prepare you nanofibers? Do you just mix the polymers and centrifuge the fibers prior of a re-suspension for NMR quantification? If you do it like this how to can you be sure that the NMR signals measured really reflect the "complete" sample. It might well be that you have a focus on polymers re-dissolved out of the fibers or that you have a focus on fibers with lower MW and that you actually do not see the real high-MW fibers in your suspension by NMR.
To clarify on this I would suspend a defined amount of fibers and quantify (in terms of mg/ml) this amount by NMR. Only if the NMR determined amount is in reasonable agreement with the amount you suspended I would trust the integrals of the different chemical groups and belief that the ratios of polymers determined provide the "full picture".
DOSY might also be helpful to clarify whether all NMR show "infinitely slow" diffusion - which I guess is expected for nano-fibers.
For solid-state NMR the literature cited by Abdelkader BOUAZIZ (thanks for this reference!) is definitely a way to go. But I think the method described is not trivial and not readily available in any NMR group.
I hope this helps
Alfred
P.S. Is it possible to re-dissolve harvested nano-fibers into their components by a suited solved. In this case quantification of the polymers in such a sample would be straight forward.
Yes, it's possible. To answer your question, do the followings :
1)Before making the fibers, run the individual NMR spectra of PCL (spectrum A) , PLGA (spectrum B ) and of their 50:50 mixture ( spectrum MIX ) in a common solvent ( call it SLV ) .) .
2) Make the fibers
3) Dissolve the fibers in solvent SLV, and run the NMR (spectrum FIB ) ;
4) Compare the spectrum of the 50:50 mixture (spectrum MIX) with the spectrum of the fiber solution (spectrum FIB), If no unexpected event took place in Stage 2 above, then Spectrum MIX must be identical to Spectrum FIB . If not identical, then the 50:50 ratio is not present in the fibers.