Assessment of Homogeneity of Elemental Mass Fractions in a Castor Leaf ( Ricinus communis L.) Reference Material Candidate Using ANOVA and PCA

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ID: 314552
2026
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Abstract
Abstract Background Certified reference materials (CRMs) are essential for method validation, quality control, and metrological traceability in analytical chemistry. However, CRMs for plant matrices of regional relevance, such as castor bean (Ricinus communis L.) leaves, remain scarce in tropical and subtropical regions. This study addresses that gap by evaluating the homogeneity of a castor bean leaf RM candidate produced under single-laboratory conditions. Objective To assess between- and within-unit homogeneity of a Ricinus communis L. leaf RM candidate for seven inorganic elements (Al, Ca, Cu, Fe, Mg, P and Zn), following ISO Guide 35:2017. This study does not aim at certification or replacement of full certification procedures as specified in ISO 17034:2016. Methods Castor bean leaf samples were collected in Bahia, Brazil. A total of 400 g of dry material was produced, homogenized, and distributed among 20 units. Elemental mass fractions were determined by microwave-induced plasma optical emission spectrometry (MIP OES) after acid digestion. Data were evaluated by one-way ANOVA (ISO Guide 35:2017) and principal component analysis (PCA) as a complementary exploratory tool. Results A minimum sample mass of 400 mg was established as adequate for reliable homogeneity evaluation. Ten units were randomly selected for between-bottle assessment, with three subsamples per unit for within-bottle evaluation. Conclusion The RM candidate was considered homogeneous for all seven elements at the 95% confidence level. PCA provided additional exploratory insights, including identification of atypical subsamples not detectable by univariate ANOVA. Highlights Castor bean RM will be of great use for confirming the accuracy of methods, which will facilitate the validation of analytical methods and verification of quality control of samples of vegetable leaves or similar matrix, in addition to allowing metrological traceability.
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Authors Altemar da Cruz Luciano, Adriana Costa Ferreira, Geovani C. Brandão, F bio de S. Dias, E Melissa Gogliath Silva, Walter Nei Lopes dos Santos, Liz Oliveira dos Santos
Journal journal of aoac international
Year 2026
DOI
10.1093/jaoacint/qsag042
URL
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