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LC condition to separate Methyl salicylate and Methylparaben

Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.

3 posts Page 1 of 1
Hi everyone,

I had a new project to assay content of Methyl paraben in Methyl salicylate cream. I faced some problem after inject methyl salicylate. I found some unknown peak at the same RT with methyl paraben. Is it possible to have a methyl paraben in methyl salicylate? and is it possible to have peak elute at the same RT with same DAD profiles?

Thank you

Jay
Yes. Structurally they are similar since the hydroxyl group is meta and the other is para. Both are methyl esters of the terminal car
Hi everyone,

I had a new project to assay content of Methyl paraben in Methyl salicylate cream. I faced some problem after inject methyl salicylate. I found some unknown peak at the same RT with methyl paraben. Is it possible to have a methyl paraben in methyl salicylate? and is it possible to have peak elute at the same RT with same DAD profiles?

Thank you

Jay
boxyl group.

Your LC method must be able to separate these esters and separate them based on the location of the hydroxyl group (they are likely to be impurities of one another). I would also assume the DAD profiles to be very similar since FTIR/IR is used to routinely differentiate between meta and para esters.
Stuff like this was my job for over 4 decades!

We also assayed methyl paraben by capillary GC after DMF extraction and BSTFA derivatization, but sounds like you do not want to go that route. We've also assayed methyl salicylate by GC as well.

I assume that you're using a detection wavelength of about 280nm, and that you've run the assay out more minutes to demonstrate that your unknown contribution is simply not from a previous injection. And I assume that you have an acidic mobile phase, acidified with some acetic acid, phosphoric acid, or a buffer.

I also assume that you have reduced the injection volume and the co-elution is the same.
So - the easiest thing would be to make standard mix of methyl salicylate and methyl paraben and vary HPLC conditions, start with one parameter at a time, and make note of whether the separation gets better, worse, or stays the same. Maybe the easiest thing to try is to change the temperature of the column by 10C or 20C.

If a temperature change seems to help, investigate mobile phase changes, like more or less organic, changing organic from methanol to ACN or HPLC ethanol (don't know what you're using now), or even adding a wee bit of non-UV THF to the mix, can do wonders.

Flow rate changes won't change things much; if your assay is isocratic, consider doing a gradient.

Trying a different phase column from same or different manufacturer could help.

This is the fun stuff, enjoy the process. This reminds me of a more common assay issue with methyl paraben - close or co-elution with phenoxyethanol - that I solved like 2 decades ago....

Or hire me as consultant!
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