Development and production of certified reference material of sugarcane leaves for assessment of nutritional quality

Author(s)

Maria Isabel Vega Martinez

• Document type: Doctoral Thesis
• Press: Piracicaba.
• Institution: Universidade de São Paulo (USP). Centro de Energia Nuclear na Agricultura (CENA/STB)
• Defense date: 2016-04-29

Examining board members

Elisabete Aparecida De Nadai Fernandes; José Lavres Junior; Ana Rita de Araujo Nogueira; Pedro Vitoriano de Oliveira

• Advisor: Elisabete Aparecida De Nadai Fernandes

Abstract

The sugarcane and derived products are of great economic importance for Brazil and several other countries. Many varieties of sugar cane are grown and new varieties have been developed to seek productivity gains. In this sense, certified reference materials (CRMs) are necessary for the quality control of measurement systems and validation of methods, aiming at the study of the nutritional status of the different sugarcane varieties for optimizing fertilization and increasing production. However, according to the international database of certified reference materials (COMAR) there is not a suitable CRM for the assessment of nutritional status of sugarcane. Thus, this work investigates the possibility of producing a reference material from leaves of sugarcane to fulfill such a demand. The work was divided into two main steps: 1) study of sugarcane varieties regarding elemental composition and 2) development of the reference material. Twelve varieties of sugarcane grown in the State of São Paulo were covered in the study: CTC2, CTC4, CTC11, CTC14, CTC15, CTC17, CTC20, IACSP955000, RB855156, RB965902, RB966928 and SP832847. The analytical techniques used for the assessment of composition were neutron activation analysis (NAA) and optical emission spectrometry with inductively coupled plasma (ICP OES), in addition to the Kjeldahl method for determination of N. In general, the results showed macronutrients in adequate levels, while, among the micronutrients, Cu and Zn were found in the critical limit for almost all the varieties studied. The selection of the variety RB966928 for producing the candidate reference material was based on the nutritional characteristics for high productivity, on the lower coefficients of variation of sampling in the field (RSD < 30%) and on the agronomic characteristics. The candidate material was produced from 90 kg of leaves, using only 15 cm from the central part without the main rib. After various tests for determining the best preparation procedure, the leaves were lyophilized, milled and homogenized, obtaining 410 bottles of the candidate material containing 20 g each. The physical characterization found residual moisture of 3.8 % and particle size < 115 µm. Homogeneity tests within and between bottles were performed using NAA and Kjeldahl method. The results confirmed the within bottle homogeneity of the material for all eighteen elements, using masses from 180 mg to 200 mg, while the homogeneity between bottles was confirmed for twenty elements. Stability studies in the short and the long term demonstrated that the material was stable in the three conditions used (40°C with a relative humidity of 100%, 20°C and 20°C). The final characterization of the candidate material was performed at NIST, National Institute of Standards and Technology, United States, where values were assigned for eighteen elements with respective expanded uncertainties: Al, Br, Ca, Ce, Cl, Co, Cs, Fe, K, La, Mg, Mn, Na, Rb, Sc, Sm, Th, and Zn. In addition, estimated values were also assigned for Hf, N, P, Sb, Sr and V determined by the Kjeldahl method and INAA (AU)

• FAPESP's process: 11/21675-0 - Development and production of certified reference material of sugarcane leaves for evaluation of nutritional quality
• Grantee: Maria Isabel Vega Martinez
• Support Opportunities: Scholarships in Brazil - Doctorate