[kriggy]

Hi there guys,
as a part of my thesis I will be studing reaction mechanism using HPLC-MS but I´ve never done anything even remotely similar to this so I was looking for some literature which can help me understand how it is done (how to interpret data from HPLC-MS). I was trying to find some articles but I wasnt succesful so far..
Does anyone has any experience with this kind of stuff ? What should I look for?

[discodermolide]

Well the MS will provide you with a molecular ion and a fragmentation pattern, then you can make an educated guess as to the structure, especially if you know the starting materials and reagents.
The LC will allow you to run the reaction and follow it on a time axis so you can see the build up of products and consumption of starting materials. Also if you use a calibrated LC (quantitative) you can work out some reaction kinetics.
Remember to run your starting materials through the system to collect all the data.

[kriggy]

Does it work for rearangement reactions? The reaction was supposed to be reduction of diazonium salt by sodium sulfite but instead of reduction the was some kind of cyclization to form 5-membered cycle but the only difference in mollar mass between starting material and product is the sulfite group which get cleaved.
I know the starting material and product.
Do you have any literature regarding this topic?

Thank you very much for help

[discodermolide]

Provided you can separate them by LC it should work. The MS fragmentation of the product should be different from that of the SM. Experiment, put both of them singly and together through the system and see what you get.
No literature but that's the way I would start to do this.