Rapid method for determination of protein content in cereals and oilseeds: validation, measurement uncertainty and comparison with the Kjeldahl method

Abstract

The objective of this research was to test suitability of the Dumas combustion method to completely substitute the Kjeldahl method in routine laboratory determination of crude protein content in cereals and oilseeds. The validation of the method demonstrated that it is able to determine crude protein content in cereals and oilseeds in an efficient and accurate manner, with a detection limit w(N) = 0.006%, quantification limit w(N) = 0.019%, repeatability precision RSD r = 0.41%, intra-laboratory reproducibility precision RSD R = 0.74%, trueness, expressed in terms of bias b = 0.43%, and linear response between (2.36–19.2) mg N. Measurement uncertainty, expressed as relative expanded uncertainty (coverage factor k = 2, confidence level 95%), was calculated from validation data (U rel = 2.24%). In order to examine the relationship between two methods, 15 cereal grain and oilseed samples were analyzed using Dumas and Kjeldahl procedure. The Kjeldahl procedure gave slightly lower w(N) values than the Dumas procedure: w K(N) = 0.9905 w D(N) = 0.0376 (R 2 = 0.9996). Relative standard deviations and results of homogeneity test obtained during analysis of complex cereal products (cereal breakfast and muesli bars) show that the Dumas combustion method may be less suitable for analysis of such samples compared to Kjeldahl method.