Food Analytical Methods

, Volume 13, Issue 1, pp 69–77 | Cite as

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

  • Raimundo R. Gamela
  • Vinícius C. Costa
  • Edenir R. Pereira-FilhoEmail author


In the present study, a simple and fast procedure using ultrasound-assisted extraction was developed for the determination of Ca, Fe, K, Mg, Mn, P, and Zn in pepper samples by inductively coupled plasma optical emission spectrometry (ICP OES). For the optimization of variables, the procedure used was the factorial design (23) and the conditions evaluated and optimized were concentration of nitric acid (1 mol L−1), sonication time (5 min), and sonication temperature (40 °C). A certified reference material (CRM) of tomato leaves (NIST 1573a) was used to evaluate the accuracy of the developed procedure by ultrasound-assisted extraction. The obtained concentration values were concordant with the certified values based on Student t test at 95% of confidence level. Therefore, the optimized conditions were applied to determine the analytes in five pepper samples, and the concentration values ranged between 1639 and 4861 mg kg−1 (Ca), 51 and 196 mg kg−1 (Fe), 558 and 13,050 mg kg−1 (K), 553 and 1662 mg kg−1 (Mg), 7 and 46 mg kg−1 (Mn), 2306 and 3793 mg Kg−1 (P), and 8–21 mg kg−1 (Zn).


Factorial design Ultrasound-assisted extraction ICP OES Pepper samples 



The authors acknowledge the financial support of the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), World Academy of Science (TWAS, process number 158587/2017-0), and Fundação de Amparo à Pesquisa do Estado de São Paulo Bahia (FAPESP, process number 2016/01513-0). This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior—Brasil (CAPES)—Finance Code 001.

Compliance with Ethical Standards

Conflict of Interest

Raimundo R. Gamela declares that he has no conflict of interest. Vinícius Câmara Costa 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.

Supplementary material

12161_2019_1524_MOESM1_ESM.docx (15 kb)
ESM 1 (DOCX 15 kb)


  1. Abuajah CI, Ogbonna AC, Osuji CM (2014) Functional components and medicinal properties of food: a review. J Food Sci Technol 52:2522–2529. CrossRefPubMedPubMedCentralGoogle Scholar
  2. Agostini-Costa TS, Gomes IS, de Melo LAMP, Reifschneider JB, Ribeiro CSC (2017) Carotenoid and total vitamin C content of peppers from selected Brazilian cultivars. J Food Compos Anal 57:73–79CrossRefGoogle Scholar
  3. Amorim FAC, Costa VC, Silva EGP, Lima DC, Jesus RM, Bezerra MA (2017) Multivariate optimization of simple procedure for determination of Fe and Mg in cassava starch employing slurry sampling and FAAS. F Chem 227:41–47. CrossRefGoogle Scholar
  4. Bae H, Jayaprakasha GK, Jifon J, Patil BS (2012) Variation of antioxidant activity and the levels of bioactive compounds in lipophilic and hydrophilic extracts from hot pepper (capsicum spp.) cultivares. Food Chem 13:1912–1918CrossRefGoogle Scholar
  5. Batista EF, Augusto AS, Pereira-Filho ER (2016) Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to used by adults and children. Talanta 150:206–2012CrossRefGoogle Scholar
  6. Belitz H-D, Grosch W, Schieberle P (2004) Food chemistry 3rd revised ed. Springer Berlin, HeidelbergCrossRefGoogle Scholar
  7. Bezerra MA, Ferreira SLC, Novaes CG, dos Santos AMP, Valasques GS, Cerqueira UMFM, Alves JPS (2018) Simultaneous optimization of multiple responses and its application in analytical chemistry-a review. Talanta 194:941–959. CrossRefPubMedGoogle Scholar
  8. Boschetti W, Rampazzo RT, Dessuy MB, Vale MG, de Oliveira Rios A, Hertz P, Manfroi V, Celso PG, Ferrão MF (2013) Detection of the origin of Brazilian wines based on the determination of only four elements using high-resolution continuum source flame AAS. Talanta 111:147–155. CrossRefPubMedGoogle Scholar
  9. Bressy FC, Brito GB, Barbosa IS, Teixeira LSG, Korn MGA (2013) Determination of trace element concentrations in tomato sample at different stages of maturation by ICP OES and ICP-MS following microwave- assisted digestion. Microchem J 109:145–149CrossRefGoogle Scholar
  10. Candioti LV, De 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. CrossRefGoogle Scholar
  11. Costa VC, Guedes WN, Santos AS, Nascimento MM (2018a) 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. CrossRefGoogle Scholar
  12. Costa VC, Silva EGP, Lima DC, Franco M, 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. CrossRefGoogle Scholar
  13. D’Archivio AA, Giannitto A, Maggi MA, Ruggieri F (2016) Geographical classification of Italian saffron (Crocus sativus L.) based on chemical constituents determined by high-performance liquid-chromatography and by using linear discriminant analysis. Food Chem 212:110–116. CrossRefPubMedGoogle Scholar
  14. Damodaran S, Fennema, OR, Parkin, KL (2010) Química de alimentos de Fennema. Artmed, 4 ed. Porto AlegreGoogle Scholar
  15. Emboscado ME (2015) Spices and herbs: natural sources of antioxidants-a mini review. J Funct Foods 18:811–819. CrossRefGoogle Scholar
  16. European Food Safety Authority- EFSA (2006) Tolerable upper intake levels for vitamins and minerals. Accessed 23 November 2018
  17. Ferreira SLC, Korn MGA, Ferreira HS, da Silva EGP, Araújo RGO, Souza AS, Macedo SM, Lima DC, de Jesus RM, Amorim FAC, Bosque-Sendra JM (2007) Appliacation of multivariate tecniques in optimization of spectroanalytical metods. Appl Spectrosc Rev 42:475–491. CrossRefGoogle Scholar
  18. Ferreira SLC, Miró M, da Silva EGP, Matos GD, dos Reis PS, Brandao GC, dos Santos WNL, Duarte AT, Vale MGR, Araujo RGO (2010) Slurry sampling—an analytical strategy for the determination of metals and metalloids by spectroanalytical techniques. Appl Spectrosc Rev 45:44–62. CrossRefGoogle Scholar
  19. Ferreira SLC, Junior MMS, Felix CSA, da Silva DLF, Santos AS, Neto JHS, de Souza CT, Junior RAC, Souza AS (2019) Multivariate optimization techniques in food analysis-a review. Food Chem 273:3–8. CrossRefGoogle Scholar
  20. Frena M, Quadros DPC, Castilho INB, de Gois JS, Borges DLG, Bernhard W, Madureira LAS (2014) A novel extraction-based procedure for the determination of trace elements in estuarine sediment samples by ICP-MS. Microchem J 117:1–6. CrossRefGoogle Scholar
  21. Gamela RR, Duarte AT, Barrera EG, Welz B, Dessuy MB, da Silva MM, Vale MGR (2017) Development of analytical methods for the determination of copper and manganese in infant formula using high resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis. Anal Methods 9:2321–2327. CrossRefGoogle Scholar
  22. Gamela RR, Barrera EG, Duarte AT, Boschetti W, da Silva MM, Vale MGR, Dessuy MB (2019) 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. CrossRefGoogle Scholar
  23. Karadas C, Kara D (2012) Chemometric approach to evaluate trace metal concentrations in some spices and herbs. Food Chem 130:196–202. CrossRefGoogle Scholar
  24. Khan N, Choi JY, Nho EY (2014) Determination of minor and trace elements in aromatics spices by micro-wave assisted digestion and inductively coupled plasma-mass spectrometry. Food Chem 158:200–206. CrossRefPubMedGoogle Scholar
  25. 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. CrossRefGoogle Scholar
  26. 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 PauloGoogle Scholar
  27. Leão DJ, Junior MMS, Junior JBS, de Oliveira DAF, Queiroz AFS, Ferreira SLC (2016) Ultrasound-assisted extraction for the determination of mercury in sediment samples employing cold vapor atomic absorption spectrometry. Anal Methods 8:6554–6559. CrossRefGoogle Scholar
  28. Lima AF, Lima FF, Richter EM, Munoz RAA (2016) Combination if sonication and heating for metal extraction form inorganic fertilizers prior to microwave-inudced plasma spectrometry determinations. Appl Acoust 103:124–128. CrossRefGoogle Scholar
  29. Manutsewee N, Aeungmaitrepirom W, Varanusupakul, Imyim A (2007) Determination of Cd, Cu, and Zn in fish and mussel by AAS after ultrasound-assisted acid leaching extraction. Food Chem 101:817–824. CrossRefGoogle Scholar
  30. Materska M, Perucka I (2005) Antioxidant activity of the main phenolic compounds isolated from hot pepper fruit (capsicum annuum L.). J Agric Food Chem 9:1750–1756CrossRefGoogle Scholar
  31. Millour S, Noel L, Kadar A, Chekri R, Vastel C, Guérin T (2011) Simultaneous analysis of 21 elements in foodsuffs by ICP-MS after closed-vessel microwave digestion: method validation. J Food Compos Anal 24:111–120. CrossRefGoogle Scholar
  32. Mir-marqués A, Cervera ML, De GM (2016) Mineral analysis of human diets by spectrometry methods. Trends Anal Chem 82:457–467. CrossRefGoogle Scholar
  33. Muller EI, Souza JP, Muller CC, Muller ALH, Mello PA, Bizzi CA (2016) Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk by ICP OES and ICP-MS. Talanta 156-157:232–238. CrossRefPubMedGoogle Scholar
  34. Nascentes CC, Korn M, Arruda MA (2001) A fast ultrasound-assisted extraction of Ca, Mg, Mn and Zn from vegetables. Microchem J 69:37–43. CrossRefGoogle Scholar
  35. Novaes CG, Bezerra MA, da Silva EGP, dos Santos AMP, Romão ILS, Neto JHS (2016) A review of multivariate designs applied to the optimization of methods based on inductively coupled plasma optical emission line. Microchem J 128:331–346CrossRefGoogle Scholar
  36. Oscan M (2004) Mineral contents of some plants used as condiment in Turkey. Food Chem 84:437–400. CrossRefGoogle Scholar
  37. Oscan MM, Akbulut M (2007) Estimation of mineral, nitrite and nitrite contents of medicinal and aromatic plants used as spices, condiments and herbal tea. Food Chem 106:852–858. CrossRefGoogle Scholar
  38. Pereira FMV, Pereira-Filho ER (2018) Aplicação de programa computacional livre em planejamento de experimentos: um tutorial. Quim Nova 41:1061–1071. CrossRefGoogle Scholar
  39. Santos WPC, Castro JT, Bezerra MA, Fernandes AP, Ferreira SLC, Korn MGA (2009) Application of multivariate optimization in the development of an ultrasound-assisted extraction procedure for multielemental determination in bean seeds samples using ICP OES. Microchem J 91:153–158. CrossRefGoogle Scholar
  40. Santos DCMB, Carvalho LSB, Lima DC, Leão DJ, Teixieira LSG, Korn MGA (2014) Determination of micronutrient minerals in coconut milk by ICP OES after ultrasound-assisted extraction procedure. J Food Compos Anal 34:75–80. CrossRefGoogle Scholar
  41. 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. CrossRefGoogle Scholar
  42. Soylak M et al (2004) Comparison of microwave, dry and wet digestion procedures for the determination of trace metal contents in spice samples produced in Turkey. J Food Drug Anal 12:254–258Google Scholar
  43. Sun T, Xu Z, Wu CT, Janes M, Prinyawiwatkul W, No HK (2007) Antioxidant activities of different colored sweet bell peppers (capsicum annuum L.). J Food Sci 72:S98–S102CrossRefGoogle Scholar
  44. Tadeo JL, Sánchez-brunete C, Albero B, García-valcárcel AI (2010) Application of ultrasound-assisted extraction to the determination of contaminants in food and soil samples. J Chromatogr A 1217:2415–2440. CrossRefPubMedGoogle Scholar
  45. Tiwari BK (2015) Ultrasound: a clean, green extraction technology. Trends Anal Chem 71:100–109. CrossRefGoogle Scholar
  46. Vale MGR, Oleszczuk N, dos Santos WNL (2006) Current status of direct solid sampling for electrothermal atomic absorption spectrometry—a critical review of the development between 1995 and 2005. Appl Spectrosc Rev 41:377–400. CrossRefGoogle Scholar
  47. Villa JEL, Pereira CD, Cadore S (2015) A novel, rapid and simple acid extraction for multielemental determination in chocalate bars. Microchem J 121:199–204. CrossRefGoogle Scholar
  48. Zand N, Chowdhry BZ, Zotor FB, Wray DS, Amuna P, Pullen FS (2011) Essential and trace elements content of commercial infant foods in the UK. Food Chem 128:123–128. CrossRefPubMedGoogle Scholar

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© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Group for Applied Instrumental Analysis, Department of ChemistryFederal University of São CarlosSão CarlosBrazil

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