-
- Posts: 172
- Joined: Tue May 30, 2017 6:53 am
Anybody know how to go about validating a kjedahl method
ie ICH guidelines , accuracy linearity etc or not applicable here
simple intermediate precision with 2 analyst perhaps ?
Discussions about sample preparation: extraction, cleanup, derivatization, etc.
HPLC chemist wrote:
Why are you trying to validate the Kjeldahl method? As I recall it is used for feeds, foods, and water (TKN or Total Kjeldahl Nitrogen)!
It's not an impurity method, so I don't think you'd need to have your linearity cover that far. You could probably get away with the typical 80-120%. If you want an expanded range, 50-150%. Duplicate, triplicate, or a single curve is up to you and your internal SOPs.ydna1977 wrote:
Linearity - weigh 30-120% of typical sample as detailed in method
prepare in duplicate ?
Yes, that would be how we did it. Alternatively per ICH Q2(R1), you can determine accuracy using a known reference standard so if you can find one where the percent nitrogen has been determined, you can show that you get the same result (or reasonably close based on analytical variability) using this method.ydna1977 wrote:
Accuracy - 80,100, 120% level ? amounts of acetanilide ?
in triplicate ?
Blazer wrote:It's not an impurity method, so I don't think you'd need to have your linearity cover that far. You could probably get away with the typical 80-120%. If you want an expanded range, 50-150%. Duplicate, triplicate, or a single curve is up to you and your internal SOPs.ydna1977 wrote:
Linearity - weigh 30-120% of typical sample as detailed in method
prepare in duplicate ?Yes, that would be how we did it. Alternatively per ICH Q2(R1), you can determine accuracy using a known reference standard so if you can find one where the percent nitrogen has been determined, you can show that you get the same result (or reasonably close based on analytical variability) using this method.ydna1977 wrote:
Accuracy - 80,100, 120% level ? amounts of acetanilide ?
in triplicate ?
Separation Science offers free learning from the experts covering methods, applications, webinars, eSeminars, videos, tutorials for users of liquid chromatography, gas chromatography, mass spectrometry, sample preparation and related analytical techniques.
Subscribe to our eNewsletter with daily, weekly or monthly updates: Food & Beverage, Environmental, (Bio)Pharmaceutical, Bioclinical, Liquid Chromatography, Gas Chromatography and Mass Spectrometry.