By Anonymous on Saturday, August 3, 2002 - 11:20 pm:
Dear all,
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!
Regards,
Frank
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.
Regards,
Frank
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.
814-359-3441
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.
Regards,
Mark
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.
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