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Validation of an analytical procedure – control of residual 8 solvents in a pharmaceutical substance

Aleksandra Groman ,  Agata E. Kamieńska-Duda 

Pharmaceutical Research Institute (IF), Rydygiera 8, Warszawa 01-793, Poland


            Residues of methanol, n-pentane, ethanol, tert-butylamine, 2-propanol, acetonitrile, dichloromethane and toluene were determined by headspace gas chromatography with the use of flame-ionization detector and DB-624 (60 m long, 0.32 mm ID) column. Oven temperature in headspace was 100° C for 30 min.

           According to the European Agency for the Evaluation of Medicinal Products it is considered that amount of said solvents in pharmaceutical product must not exceed:
methanol 3000 ppm, n-pentane 5000 ppm, ethanol 5000 ppm, 2-propanol 5000 ppm, acetonitrile 410 ppm, dichloromethane 600 ppm, and toluene 890 ppm.

Specification limit has been established for tert-butylamine at the level of 1000 ppm.

            Validation of the method included: selectivity, specificity, system precision, method precision, intermediate precision, accuracy (recovery), linearity, limits of detection and quantitation (in substance), robustness.


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Related papers

Presentation: Poster at VI Multidyscyplinarna Konferencja Nauki o Leku, by Aleksandra Groman
See On-line Journal of VI Multidyscyplinarna Konferencja Nauki o Leku

Submitted: 2008-03-26 10:37
Revised:   2009-06-07 00:48