Repeatability and reproducibility of determination of the nitrogen content of fishmeal by the combustion (Dumas) method and comparison with the Kjeldahl method: interlaboratory study.
Ten fishmeal samples (hidden duplicates of 4 meals plus 2 high-protein meals as a Youden pair), tryptophan, and nicotinic acid were analyzed by 18 laboratories using the Dumas method. Thirteen of the laboratories also analyzed the same 12 samples using their current Kjeldahl method. Recoveries (+/-SR) of tryptophan and nicotinic acid were 99.3+/-1.04 and 98.8+/-2.11% by Dumas and 97.1+/-3.03 and 74.6+/-26.76% by Kjeldahl. The Dumas method gave significantly greater values (P < 0.001) than the Kjeldahl method. For fishmeals, Kjeldahl N = 0.989 of Dumas N (P < 0.001). A similar proportionate difference (0.984 of Dumas N) was observed with tryptophan. Most laboratories failed to determine nicotinic acid correctly by Kjeldahl. For fishmeals, the relative standard deviations for repeatability and reproducibility were for Dumas 1.48 and 2.01% and Kjeldahl 1.62 and 2.37%, respectively. A single analysis conducted in 2 laboratories should not differ by more than 5.63% of the mean value when measured by Dumas or by more than 6.64% by Kjeldahl. It is concluded that with fishmeal, Dumas gives a more reliable measure of organic nitrogen than Kjeldahl, and, therefore, Dumas should be the method of choice.
Miller
Eric L
EL
Department of Veterinary Medicine, University of Cambridge, Cambridge, CB3 OES United Kingdom. elm1@cam.ac.uk
Bimbo
Anthony P
AP
Barlow
Stuart M
SM
Sheridan
Berni
B
D002623:Chemistry Techniques, Analytical / Q000379:methods; D005396:Fish Products / Q000032:analysis*; D009584:Nitrogen / Q000032:analysis*; D015203:Reproducibility of Results
D009584:Nitrogen