GC-HS residual solvent

[AHSJ1269]

i got extra peaks in residual solvent analysis in sample run i.e. other than diluent peaks and known standard peaks

what i have to do ?

[Johnny Rod]

Identify and then quantify! Use GC-MS if you can. If not, look up your GC column in a catalogue and see which solvents they could be from the order of elution in the examples, then try a mixture to look for RT matches.

[krickos]

As indicated use standard/pharmacopiea method to identify, preferbly by MS detection.

Do not overlook the possibillity that:
a. the sample contains other residual solvents in trace amounts than stipulated on a CoA. ie check all solvents used in production.
b. sample/pH causes some sidereactions with certain aprotic solvents as DMF etc
c .headspace oven is set too high causing degradation/intercations

[chromatographer1]

Repeat sample and confirm the amount of the peaks. If they differ the sample may have been contaminated in storage, or shipping, or by an accident.

The lab air could have been the source of these peaks. Likewise the dissolution solvent may have been contaminated.

best wishes,

Rod