I have to determine solubility of LC-MS of completely new compound, however, the sample provided is very low. So, I would like to know what is the safe concentration to start.
The best to approximate the solubility by a software like ACD/Labs, Toronto, Canada and use a concentration in the analytical method at the limit of quantitation or 10x LOQ for better accuracy.
It depends on the instrument. Your reading must be in the LDR. Read the user manual for for more information. It should clearly tell you the most safe range
You probably don’t know the LOQ and LDR yet for this completely new compound yet, right?
If what matters is to know if the compound’s solubility is above certain threshold, you can simply test at this threshold level to get the answer.
For quantitation, you need to make calibration standards, which require accurate measurements (weighing or pipetting). This becomes trickier with too little material. There are ways to deal with the situation, with some compromises, of course. You will need a little thinking and planning.
Is the sample neat or a solution, e. g. a DMSO stock?