I have synthesized G0 PAMAM dendrimer. Now I have a challenge with its purification. One method is washing the product with cold Diethylether solvent. The problem is that I don’t know the detail of this method so I cannot reach a pure product. Can someone help me in this case? The MASS and NMR Spectra of this product are shown below.
Another question is that how can I measure the percent of product purification?
note: the MW of Go PAMAM is 517 and i don't have Dialysis bag with this cutoff.
Perhaps you should rethink your synthetic approach. Take a look at this recent open source review paper
Article Recent Advances in Click Chemistry Applied to Dendrimer Synthesis
Dear Maryam Behroozi,
You can follow the next procedure which is due to " Best practices for purification and characterization of PAMAM dendrimer.
Dendrimer purification:
Methanol was removed from a solution of Lot A Biomedical Grade G5 Dendrimer under reduced pressure to produce a viscous oil. The dendrimer was redissolved in water and then lyophilized to obtain a dry weight (5.1310 g). The dry dendrimer was dissolved with 80 ml of DI water and divided into 4 aliquots (Aliquots 1, 2, 3, and 4). Four 10,000 MWCO dialysis membranes were prepared with a length of approximately 14 inches. Weighted clips were attached to one end of each dialysis tube and 20 mL of the dendrimer/water solution were added to each dialysis membrane tube. Residual air was removed from each tube and the tubes were sealed with floating clips, attached so that the length of each dialysis tube was approximately 7 inches. A foam float was affixed to each of the floating clips and the dialysis tubes and placed into glass jars filled with one gallon of Nanopure water each. Slow stirring was utilized. Nanopure water was exchanged 9 times over 3 days. The minimum time between exchanges was 3 hrs. After purification, the dendrimer was removed from the dialysis tubes and placed in glass scintillation vials. The purified dendrimer (Purified Aliquots 1, 2, 3 and 4) was lyophilized for 3 days to yield 5.0238 g (98%) of a glassy material. The dried product was stored under nitrogen at −25 °C.
See the ref: Macromolecules. 2012 June 26; 45(12): 5316–5320. DOI:10.1021/ma300485p.
Best regards.
Instead of washing with diethyl ether, Take the product in round bottom flask, Add to this cold Diethyl ether and stirred it at cold condition half an hour and filter. If you do this two to three times you may get pure product.
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