N Nitroso Vildagliptin amide

Hello,

One more Nitrosamine realted to vildagliptin, whether is it consider as a NDSRI ?

We are trying to develop the LCMS method but found challenge to get specificity and Accuracy.
Such problem observed by any one ?

Thanks

@Mahendra.vaghela, based on my own experience and what I’ve seen in other cases from literature and official compendia, I can give you a general answer.

  1. When it comes to the extracted ion chromatograms (EIC), they use an m/z extraction window of ±15 ppm for quantification;
  2. Make sure that the ratio between the peak area of the main transition and the peak area of the qualifier transition for the test solution is within 20 per cent of the same ratio calculated for the spiked solution;
  3. Pay special attention to the collision-induced dissociation in the source. It can be tricky and cause confusion, messing up the real m/z value you want to isolate.

Have you checked these items?

Thanks for suggestion, we did exercise as suggested, we are trying…