Methylene Blue NDSRI

Does anyone work on Quantification of N-desmethyl-N-nitroso-methylene blue NDSRI in methylene Blue on LCMS/MS ?
We tried to develop the method for the NDSRI but we are getting recovery higher side. Tried various diluents but not succeed.

Thanks
Vivek

thanks for sharing , May i know your selection of solvent and LCMS ion precursor type

Mobile phase
0.1% TFA in Water
0.1% TFA in Methanol
Diluent mix of both
LCMS ion precursor type ESI+ mass 299.3
Fragment 269.2 & 252.2

Hi, Have you tried to increase the sample concentration

Yes, If we increase the sample conc. the impurity also increasing. In as such sample impurity is coming near LOQ level.

Just for context…

SMILES: CN(C)c1ccc2c(c1)sc-3cc(=N+C)ccc3n2.[Cl-]

image

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Hello Vivek,

Good to know that you are working on this NDSRI and would be helpful which limits are applied for this NDSRI in methylene blue API