I have prepared sulfonated porphyrins and purified by soxhlet extraction. But MALDI-TOF analysis showed other impurities. I would appreciate if you could suggest me some suitable method to purify sulfonated compounds.
Compound is only soluble in water and methanol. Also, I tried to wash the compound with ether and hexane together, but formed viscous stuff and unable to recover as powder.
Solid Phase Extraction (SPE) is known as an excellent purification technique. As your sulfonated porphyrins compunds solubility only in water and methanol, then I feel C18 could be your possible choice for SPE extraction cartridge. Since, I am not aware the full chemistry of your molecule, thus you are also suggested to make SPE cartridges confirm according to your molecule. You can also use MeOH, Water, hexane, ether or their combination as mobile phase during elution of the sulfonated porphyrins molecule from the SPE cartridge.
You probably need to try some form of LC, depending on how chemically similar your side products are in comparison to the desired product. Water/Methanol gradients are commonly used in reverse phase HPLC with C4 or C18 stationary phases. There are many other options; the best choice will depend on the chemistry of the analytes you want to separate. Can you provide more information?
Thank you Md.Saddam Nawaz, Abigail Turner and Johannes Ahrens for your kind suggestions.
Nawaz and Turner: I don't have any HPLC system and I unable to use C18 column. So I should think best possible ways to purify my compound. I feel recrystallation kind of techniques should work.
Johannes Ahrens: I will try to purify the compound by your suggestion. Thanks for your kind suggestion.
Abigail Turner: For sulfonation, I used chlorosulfonic acid and neutralized with NaOH to form sulfonated salts of porphyrins. I confirmed from mass spec that there are no isomers but I feel there are inorganic salts which I need to remove.
I could notice when adding methanol to compound something is settling down (probably salts) and compound dissolves in methanol (confirmed by mass and UV). But it is not 100% pure. So please suggest how to get 100% pure compound.
Thank you in advance.
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