Proposition of Sample Preparation Procedure of Cassava Flour with Diluted Acid Using Mixture Design and Evaluation of Nutrient Profiles by Multivariate Data Analysis

  • 134 Accesses

  • 1 Citations


In this study, we evaluated the efficiency of an extraction procedure with diluted acids using a digester block. The procedure was developed for the extraction of Ca, Cu, Fe, K, Mg, Mn, P, S, and Zn in handmade cassava flour samples produced in the south and extreme southern regions of Bahia State, Brazil. A mixture design was used for the optimization of the proportions of the acid mixture used in the extraction procedure, and the optimized conditions were 3.0 mL of HNO3 (3.5 mol L−1) and 3.0 mL of HCl (3.5 mol L−1). In the south and extreme south regions were obtained twenty-two and twenty-nine cassava flour samples, respectively. The determination of the analytes was performed using an inductively coupled plasma optical emission spectrometry (ICP OES). Accuracy of the proposed procedure was evaluated from the analysis of the certified reference material (CRM) of rice flour (NIST 1568b) and the results obtained by the proposed method were statistically in agreement with the certified values. The concentration range of Ca, Cu, Fe, K, Mg, Mn, P, S, and Zn found in the samples were compared with the values of recommended dairy intake (RDI), and we concluded that cassava flour is a good nutrient source. For the evaluation and interpretation of the data, multivariate analysis using principal components analysis (PCA) was used, and the results showed a separation between the samples of the south and extreme southern regions.

This is a preview of subscription content, log in to check access.

Access options

Buy single article

Instant unlimited access to the full article PDF.

US$ 39.95

Price includes VAT for USA

Subscribe to journal

Immediate online access to all issues from 2019. Subscription will auto renew annually.

US$ 99

This is the net price. Taxes to be calculated in checkout.

Fig. 1
Fig. 2
Fig. 3


  1. Abuajah CI, Ogbonna AC, Osuji CM (2015) Functional components and medicinal properties of food: a review. J Food Sci Technol 52:2522–2529.

  2. Amorim FAC, Costa VC, Guedes WN, Sá IP, Santos MC, Silva EGP, Lima DC (2016) Multivariate optimization of method of slurry sampling for determination of iron and zinc in starch samples by flame atomic absorption spectrometry. Food Anal Methods 9:1719–1726.

  3. Amorim FAC, Costa VC, Da Silva EGP, Lima DC, De Jesus RM, Bezerra MA (2017) Multivariate optimization of simple procedure for determination of Fe and Mg in cassava starch employing slurry sampling and FAAS. Food Chem 227:41–47.

  4. ANVISA – Agência Nacional de Vigilância Sanitária. Resolução RDC n° 269, de 22 de setembro de 2005. Available in: http://portal.anvisa. MOD=AJPERES. Accessed 12 January 2019

  5. Araujo RGO, Macedo SM, Korn MGA, Pimentel MF, Bruns R, Ferreira SLC (2008) Mineral composition of wheat flour consumed in Brazilian cities. J Braz Chem Soc 19:935–942.

  6. Araújo A, Marinho W, Gomes AA (2018) A fast and inexpensive chemometric-assisted method to identify adulteration in acai (Euterpe oleracea) using digital images. Food Anal Methods 11:1920–1926.

  7. Armenta S, Garrigues S, de la Guardia M (2015) The role of green extraction techniques in green analytical chemistry. Trends Anal Chem 71:2–8.

  8. Audu AA, Waziri M, Olasinde TT (2012) Proximate analysis and levels of some heavy metals in cassava flour processed by roadside drying along Abuja-Lokoja highway, Nigeria. In: J Fund App Life Sci, vol 3, pp 55–58

  9. Bamidele OP, Fasogbon MB, Oladiran DA, Akande EO (2015) Nutritional composition of fufu analog flour produced from cassava root (Manihot esculenta) and cocoyam (Colocasia esculenta) tuber. Food Sci Nutr 3:597–603

  10. Belitz HD, Grosch W, Schieberle P (2004) Food chemistry, 3ª edn. Springer, p 1070

  11. Bendicho C, Lavilla I, Pena-Pereira F, Romero V (2012) Green chemistry in analytical atomic spectrometry: a review. J Anal At Spectrom 27:1831–1857.

  12. Bizzi CA, Pedrotti MF, Silva JS, Barin JS, Nóbrega JA, Flores EMM (2017) Microwave-assisted digestion methods: towards greener approaches for plasma-based analytical techniques. J Anal At Spectrom 32:1448–1466.

  13. Bro R, Smilde AK (2014) Principal component analysis. Anal Methods 6:2812–2831.

  14. Candioti LV, Zan MM, Cámara MS, Goicoechea HC (2014) Experimental design and multiple response optimization. Using the desirability function in analytical methods development. Talanta 124:123–138.

  15. Correia FO, Silva DS, Costa SSL, Silva IKV, Da Silva DR, Alves JPH, Garcia CAB, Maranhão TA, Passos EA, Araujo RGO (2017) Optimization of microwave digestion and inductively coupled plasma-based methods to characterize cassava, corn and wheat flours using chemometrics. Microchem J 135:190–198.

  16. Costa VC, Babos DV, Aquino FWB, Virgilio A, Amorim FAC, Pereira-Filho ER (2018a) Direct determination of Ca, K and Mg in cassava flour samples by laser-induced breakdown spectroscopy (LIBS). Food Anal Methods 11:1886–1896.

  17. Costa VC, Da Silva EGP, Lima DC, Franco M, De Jesus RM, Bezerra MA, Amorim FAC (2018b) Use of mixture design with minimal restrictions to optimize an extraction procedure employing diluted acids assisted by ultrasound and microwave for nutrient element determination in vegetal samples. J Braz Chem Soc 29:1189–1198.

  18. Costa VC, Guedes WN, Santos AS, Nascimento MM (2018c) Multivariate optimization for the development of a fast and simple ultrasound-assisted extraction procedure for multielemental determination in tea leaves by inductively coupled plasma optical emission spectrometry (ICP OES). Food Anal Methods 11:2004–2012.

  19. Da Silva IRC, Cardoso RCV, Góes JAW, Druzian JI, Vidal PO, De Andrade ACB (2017) Food safety in cassava “flour houses” of Copioba Valley, Bahia, Brazil: diagnosis and contribution to geographical indication. Food Control 72:97–104.

  20. DalCorso G, Manara A, Piasentin S, Furini A (2014) Nutrient metal elements in plants. Metallomics 6:1770–1788.

  21. De Souza CT, Soares SAR, Queiroz AFS, Dos Santos AMP, Ferreira SLC (2016) Determination and evaluation of the mineral composition of breadfruit (Artocarpus altilis) using multivariate analysis technique. Microchem J 124:84–88.

  22. Do Prado SBR, Giuntinia EB, Grandea F, De M (2016) Techniques to evaluate changes in the nutritional profile of food products. J Food Compost Anal 53:1–6.

  23. Dos Santos AMP, Oliveira AC, Souza AS, Jesus RM, Ferreira SLC (2011) Determination and evaluation of the mineral composition of Chinese cabbage (Beta vulgaris). Food Anal Methods 4:567–573.

  24. Dos Santos IF, Dos Santos AMP, Barbosa UA, Lima JS, Dos Santos DC, Matos G (2013) Multivariate analysis of the mineral content of raw and cooked okra (Abelmoschus esculentus L.). Microchem J 110:439–443.

  25. Dos Santos AMP, Santos LO, Brandao GC, Leão DJ, Bernedo AVB, Lopes RT, Lemos VA (2015) Homogeneity study of a corn flour laboratory reference material candidate for inorganic analysis. Food Chem 178:287–291.

  26. Dos Santos AMP, Lima JS, Dos Santos IF, Silva EFR, De Santana FA, De Araujo DGGR, Dos Santos LO (2019) Mineral and centesimal composition evaluation of conventional and organic cultivars sweet potato (Ipomoea batatas (L.) Lam) using chemometric tools. Food Chem 273:166–171.

  27. FAO (2015) (Food and agriculture organization of the united nations). FAOSTAT Statistics Database Rome: UN Food ande Agriculture Organization Available at Accessed 29 January 2019

  28. FDA, Food and Drug Administration (2013) Guidance for industry: a food labeling guide (14. Appendix F: Calculate the percent daily value for the appropriate nutrients), Available at Accessed 12 January 2019

  29. Ferreira SLC, Silva LOB, Santana FA, Junior MMS, Matos GD, Santos WNL (2012) A review of reflux systems using cold finger for sample preparation in the determination of volatile elements. Microchem J 106:307–310.

  30. Ferreira SLC, Silva MM Jr, Felix CSA, da Silva DLF, Santos AS, Neto JHS, de Souza CT, Cruz RA Jr, Souza AS (2019) Multivariate optimization techniques in food analysis – a review. Food Chem 273(3–8):3–8.

  31. Gamela RR, Barrera EG, Duarte AT, Boschetti W, da Silva MM, Vale MG, Dessuy MB (2019a) Fast sequential determination of Zn, Fe, Mg, Ca, Na, and K in infant formulas by high-resolution continuum source flame atomic absorption spectrometry using ultrasound-assisted extraction. Food Anal Methods 12:1420–1428.

  32. Gamela RR, Costa VC, Pereira-Filho ER (2019b) Multivariate optimization of ultrasound-assisted extraction procedure for the determination of Ca, Fe, K, Mg, Mn, P, and Zn in pepper samples by ICP OES. Food Anal Methods.

  33. Gimou MM, Charrondiere UR, Leblanc JC, Pouillot R, Noel L, Guerin T (2014) Concentration data for 25 elements in foodstuffs in Yaounde: the Cameroonian Total Diet Study. J Food Compos Anal 34:39–55.

  34. Gomes BS, Pereira Junior JB, Nunes PO, Lemos MS, Dantas Filho HA, Dantas KGF (2017) Assessment of the concentration of trace elements in cassava flour (Manihot esculenta Crantz) by inductively coupled plasma optical emission spectrometry. Rev Virtual Quim 9:1699–1711.

  35. IBGE, Instituto Brasileiro de Geografia e Estatística (2017) en/10966-asi-overweight-affects-388-million-adult-brazilians.html Accessed 29 Jan 2019

  36. Korn MGA, Morte ESB, dos Santos DCMB, Castro JT, Barbosa JTP, Teixeira AP, Fernandes AP, Welz B, dos Santos WPC, dos Santos EBGN, Korn M (2008) Sample preparation for the determination of metals in food samples using Spectroanalytical methods - a review. Appl Spectrosc Rev 43:67–92.

  37. Krug FJ, Rocha FRP (2016) Métodos de preparo de amostras. Fundamentos sobre o preparo de amostras orgânicas e inorgânicas para análise elementar. Editora, EditSBQ, São Paulo

  38. Lima DC, Dos Santos AMP, Araujo RGO, Scarminio IS, Bruns R, Ferreira SLC (2010) Principal component analysis and hierarchical cluster analysis for homogeneity evaluation during the preparation of a wheat flour laboratory reference material inorganic analysis. Microchem J 95:222–226.

  39. Oboh G, Akindahunsi A, Oshodi A (2002) Nutrient and anti-nutrient contents of Aspergillus niger-fermented cassava products (flour and Gari). J Food Compos Anal 15:617–622.

  40. Pereira FMV, Pereira-Filho ER (2018) Aplicação de programa computacional livre em planejamento de experimentos: um tutorial. Quim Nova 41:1061–1071.

  41. Santos LO, Brandão GB, Dos Santos AMP, Ferreira VAL (2016) Direct and simultaneous determination of copper and iron in flours by solid sample analysis and high-resolution continuum source graphite furnace atomic absorption spectrometry. Food Anal Methods 10:469–476.

  42. Santos HM, Coutinho JP, Amorim FAC, Lôbo IP, Moreira LS, Nascimento MM, Jesus RM (2019) Microwave-assisted digestion using diluted HNO3 and H2O2 for macro and microelements determination in guarana samples by ICP OES. Food Chem 273:159–165.

  43. Schiavo D, Trevizan LC, Pereira-Filho ER, Nóbrega JA (2009) Evaluation of the use of multiple lines for determination of metals in water by inductively coupled plasma optical emission spectrometry with axial viewing. Spectrochim Acta B 64:544–548.

  44. Schneider M, Schneider RCS, Corbellini VA, Mahlmann CM, Fior CS, Ferrão MF (2018) Exploratory analysis applied for the evaluation of yerba mate adulteration (Ilex paraguariensis). Food Anal Methods 11:2035–2041.

  45. TACO, Brazilian Table of Food Composition (2011) tabela.php/ Accessed 03 Mar 2019

  46. Tarantino TB, Barbosa IS, Lima DC, Pereira MG, Teixeira LSG, Korn MGA (2016) Microwave-assisted digestion using diluted nitric acid for multi-element determination in rice by ICP OES and ICP-MS. Food Anal Methods 10(4):1007–1015.

Download references

Author information

Correspondence to Edenir Rodrigues Pereira-Filho.

Ethics declarations

Conflict of Interest

Vinicius Câmara Costa declares that he has no conflict of interest. Fabio Alan Carqueija Amorim declares that he has no conflict of interest. Diego Victor Babos declares that he has no conflict of interest. Raimundo Rafael Gamela declares that he has no conflict of interest. Edenir Rodrigues Pereira-Filho declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies involving human participants or animals performed by any of the authors.

Informed Consent

Informed consent was obtained from all individual participants included in the study.

Additional information

This is an original research article that has neither been published previously nor considered presently for publication elsewhere. All authors named in the manuscript are entitled to the authorship and have approved the final version of the submitted manuscript.

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Electronic supplementary material

Supplementary Table 1

(DOCX 22 kb)

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Costa, V.C., Babos, D.V., Gamela, R.R. et al. Proposition of Sample Preparation Procedure of Cassava Flour with Diluted Acid Using Mixture Design and Evaluation of Nutrient Profiles by Multivariate Data Analysis. Food Anal. Methods 13, 145–154 (2020).

Download citation


  • Cassava flour
  • Nutrients elements
  • Diluted acid
  • Mixture design
  • And multivariate analysis