Problems with GC/MS Diclofenac method

Chromatography Forum: GC Archives: Problems with GC/MS Diclofenac method
Top of pagePrevious messageNext messageBottom of pageLink to this message  By tomo on Wednesday, July 28, 2004 - 04:28 am:

Firstly I know that LC or HPLC may well be more suited for this analysis.

I am having real problems in developing a Diclofenac method using GC/MS.

I am using a d4 version of Diclofenac as an internal standard. PFPA, followed by a tBDMSi derivitisation process.

I am calibrating in a range from 0.5-50ng/ml.

I have been having some very peculiar results, with 5-25ng/ml being linear. At <5ng/ml, responses leap, throwing the whole calibration curve off.

I can supply more details, such as GC temp. program, injection volume, etc. The matrix is human fluid (serum/plasma).

Reprouducibilty is also a problem.

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