In:
Journal of AOAC INTERNATIONAL, Oxford University Press (OUP), Vol. 65, No. 1 ( 1982-01-01), p. 52-61
Abstract:
A spectrophotometric analytical method for the determination of arprinocid [9-(2-chloro-6-fluorophenylmethyl)- 9H-purin-6-amine] in premixes has been evaluated in an interlaboratory collaborative study. The samples were prepared in pairs over the concentration range 10.1-16.2% arprinocid with 2 similar materials as carriers for the drug, and were distributed to 16 laboratories. Duplicate analyses were obtained within the overall paired sample design by a protocol which obviates data censoring and allows for statistical treatment according to both Youden and Steiner guidelines. Each collaborator was requested to run 1 determination on each of 16 differently numbered samples in groups of 8 on 2 different days. In this analytical procedure, the drug is extracted into CHC13 and transferred into 0.1N HC1 for measurement at 258 nm after isolation by liquid- liquid partitioning. The means of the analyses reported by the collaborators ranged from 96.9 to 101% of the true concentration of arprinocid and were not statistically significantly different (P & gt;0.1) from the true values. The coefficient of variation at the 12.2% formulation concentration level was 3.6%. The collaborative data were normally distributed (P ≮ 0.01) with a mean, median, and mode of 99.2, 99.2, and 100.0% recovery, respectively, and a standard deviation of 3.72%. In this distribution, 80% of the results were within the range 95.1-104.1% recovery. The systematic standard deviations of the 4 unit blocks (Sb) were each & lt;0.4% arprinocid and the analysis of variance demonstrated that laboratory bias is not statistically significant (P & gt;0.05). There is no statistically significant difference in either accuracy (P & gt;0.5) or precision (P & gt;0.05) between days, and the ruggedness test confirms that none of the 7 procedural variations which were selected for study has a significant effect on the analysis. This method has been adopted official first action.
Type of Medium:
Online Resource
ISSN:
0004-5756
DOI:
10.1093/jaoac/65.1.52
Language:
English
Publisher:
Oxford University Press (OUP)
Publication Date:
1982
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