Residual Solvents in Pharmaceuticals: NMP - HS or Split?

Chromatography Forum: GC Archives: Residual Solvents in Pharmaceuticals: NMP - HS or Split?
Top of pagePrevious messageNext messageBottom of pageLink to this message  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


Top of pagePrevious messageNext messageBottom of pageLink to this message  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!


Top of pagePrevious messageNext messageBottom of pageLink to this message  By frank on Monday, August 5, 2002 - 03:36 am:

Oh, sorry, NMP is N-Methylpyrrolidinone or N-Methylpyrrolidone.

Regards,

Frank


Top of pagePrevious messageNext messageBottom of pageLink to this message  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


Top of pagePrevious messageNext messageBottom of pageLink to this message  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


Top of pagePrevious messageNext messageBottom of pageLink to this message  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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