I am working in pharmaceutical company and we use NMP as solvent in the last step of the synthesis of a drug substance (= API). Therefore I want to develop a GC method for the determination of NMP in the DS. However, our standard HS-GC method for residual solvents in APIs is not sensitve enough for the detection of the ICH concentration limit for NMP (520 ppm). Does anybody know a HS-GC-method for NMP-determination in the range 100-600 ppm? Maybe split injection is an alternative. But: How can I prevent the API from entering the GC column without using a difficult and time consuming sample preparation? Is SPE an alternative? Who has experience?
Thank you all in advance!
By Anonymous on Sunday, August 4, 2002 - 04:27 pm:
I know what ICH HS-GC and SPE means but what is NMP? DS? Is API the acronym for the drug itself?
Thanks for the clarification!
By frank on Monday, August 5, 2002 - 03:36 am:
Oh, sorry, NMP is N-Methylpyrrolidinone or N-Methylpyrrolidone.
By Anonymous on Monday, August 5, 2002 - 05:55 am:
This is a less volatile analyte that may be best analyzed by headspace SPME. I would ask Supelco technical service if they could help you.
By Anonymous on Monday, August 5, 2002 - 07:35 am:
Dear original anon,
We determine this same compound for the same reason by RP-HPLC. The mobile phase is hexanesulfonate-ACN with detection at 205 nm. Works very well, has a very low quantitation limit.
By Anonymous on Monday, August 5, 2002 - 07:53 am:
We use capillary GC with split inlet and FID on HP-1 type column to determine residual toluene in an API. We dissolve the API in a non-interfering solvent, isothermal at 40 C, split injection, the API gets trapped on the split liner. Either external standard or internal standard can be used.
Posting is currently disabled in this topic. Contact your discussion moderator for more information.