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Background: Laboratory sampling is a significant source of error in feed testing. Proficiency testing programs such as the Association of American Feed Control Officials Proficiency Testing Program are an effectivemeans of assessing error in and among analyticalmethods. However, all proficiency test items are comminuted and blended to control variability among items, effectivelyminimizing sampling error. Currently there is nomechanismformonitoring sampling error among laboratories. Objective: The objective of this work was to investigate the feasibility of a proficiency testing program for laboratory sampling methods and provide insight into a program to advance the performance of sampling in laboratories. Methods: The study involved the fabrication of identical feed test items from feed ingredients and shipping the uncomminuted materials to volunteer laboratories. The volunteer laboratories followed in-house procedures for selecting test portions for routine feed tests. Tests on all the test portions for a single analyte were performed by a single laboratory, so that the variability in test results could be attributed to laboratory sampling processes to select test portions. Results: The average RSD, %, for Item A and Item B, respectively, were as follows: protein, 5.08 and 5.23; non-protein nitrogen, 8.90 and 16.6; crude fat, 3.45 and 5.67; vitamin A, 33.9 and 26.9; calcium, 21.9 and 23.6; zinc, 17.9 and 27.9; and copper, 17.4 and 27.9. Conclusion: This study suggests that a proficiency testing program for laboratory sampling is feasible with manual manufacture of the test items, and data can be used to monitor laboratory sampling proficiency and also to compare the performance of different laboratory sampling methods. Highlights: The data illustrates that each analyte has unique distributional and compositional heterogeneity, thus unique sampling error, even when multiple analytes are determined from a single test portion. [ABSTRACT FROM AUTHOR]

Background: Vitamin A test results have historically been notorious for poor repeatability and reproducibility. This problem has been discussed at length in Association of American Feed Control Officials Laboratory Methods and Services Committee meetings. Objective: The objective of this work was to assess the effect of test portion mass on the repeatability of vitamin A test results. Methods: The study was conducted in two parts. In Part I, fundamental sampling error (FSE) was determined experimentally through replicated (n = 16) vitamin A testing of three animal feed materials. The testing followed rigorous test portion selection for 10 g and 100 g test portions. In Part II, FSE calculations were made (1) using theoretical equations based on vitamin A as a liberated analyte and (2) on representing the particles in feed materials. Particle size characterization of vitamin A ingredients was estimated by microscopy and further evaluated by particle size analysis. Results: RSDs, % for vitamin A determinations ranged from 10.5-24.7, and 2.26-10.7 for 10 g and 100 g test portions, respectively. FSE calculated for Ingredient A ranged from 18.3-101% and 5.79-32.0% for 10 g and 100 g test portions, respectively, and for Ingredient B, ranged from 10.2-56.2% and 3.21-17.8% for 10 g and 100 g test portions, respectively. Conclusion: Test portion mass has a substantial impact on FSE and is an important factor in controlling the random error in vitamin A testing. FSE equations are useful to approximate minimum test portion mass. Highlights: Vitamin A method development should use theoretical predictions and experimental verification to guide test portion mass. Strategies to deal with the larger test portion masses will be key to validating new methods. [ABSTRACT FROM AUTHOR]

Background: Pesticide residues are analyzed in thousands of samples yearly by national authorities and private laboratories. Intensive research is ongoing to develop new methods or improve existing ones concentrating on extraction, cleanup, and detection techniques. Little attention has been paid to the contribution of prior steps in the determination process to overall laboratory sampling errors, though several publications demonstrate their practical importance. Consequently, the repeatability and reproducibility of the results are often reported based on the recovery tests alone. A few previous publications are cited in this paper which illustrate the magnitude of random errors derived from subsampling, comminution of analytical samples, and selection of small test portions. Objectives: We aim to call attention to the importance of considering all steps of laboratory sampling and analysis processes in calculating the combined uncertainty of results and realistic performance assessments of methods including their longterm intermediate precision. Method: Validation of laboratory sampling of large fruits is used to illustrate the recommended procedures, determination of their random error, and long-term method performance. Results: The results indicate that subsampling, comminution, and selection of test portions can be major contributors to the combined uncertainty of results. Conclusions: All these steps should be considered in estimation of random variation (uncertainty) of measured residues. Highlights: Random error of laboratory sampling for pesticide residues. Mass reduction of large crop units. Internal quality control of laboratory operations. [ABSTRACT FROM AUTHOR]