Keywords
fat-soluble vitamins
water-soluble vitamins
validation
liquid chromatography
How to Cite
Abstract
Two methodologies were proposed for determining vitamins in supplements by means of high performance liquid chromatography (HPLC): one for simultaneous determination of fat soluble vitamins (retinyl acetate, retinyl palmitate, α-tocopheryl acetate and β-carotene), and the other for the simultaneous determination of water soluble vitamins (B1, C, nicotinamide, nicotinic acid, B6 and pantothenic acid). The methodologies were validated using certified reference material SRM 3280 from NIST and vitamins standards. The limits of detection (LODs) and the limits of quantification (LOQs) ranged from 0.3 to 4.3 µg/mL and from 0.5 to 14.0 µg/mL, respectively. The recoveries of spiked vitamin standards in supplements ranged from 92 % to 109 %, and from 86 % to 108 % in the reference material. The repeatability was calculated by the relative standard deviation (RSD), with values from 0.2 % to 9.6 %. The validated methods were applied for determining vitamins A, E, B1, C, niacin, B6 and pantothenic acid in 10 multivitamin supplements samples. Both methods are suitable for determining vitamins in multivitamin supplements, and their applications will be essential, considering the urgent need for monitoring and for surveying these products.References
1. Alves SCR, Navarro F. O uso de suplementos alimentares por frequentadores de academias de Potim/SP. Rev Bras Nutr Esportiva. 2010;4(20):139-46.
2. Fayh APT, Silva CV, Jesus FRD, Costa GK. Consumo de suplementos nutricionais por frequentadores de academias da cidade de Porto Alegre. Rev Bras Ciênc Esporte. 2013;35(1):27-37. [DOI: 10.1590/S0101-32892013000100004].
3. Brasil. Ministério da Saúde. Resolução RDC nº 27, de 6 de agosto de 2010. Dispõe sobre as categorias de alimentos e embalagens isentos e com obrigatoriedade de registro sanitário. Diário Oficial [da] República Federativa do Brasil. Brasília, DF, 9 ago. 2010.
4. Abe-Matsumoto LT, Sampaio GR, Bastos DHM. Suplementos vitamínicos e/ou minerais: regulamentação, consumo e implicações à saúde. Cad Saúde Pública. 2015;31(7):1371-80. [DOI: 10.1590/0102-311X00177814].
5. Blake CJ. Status of methodology for the determination of fat-soluble vitamins in foods, dietary supplements, and vitamin premixes. J AOAC Int. 2007;90(4):897-910.
6. Blake CJ. Analytical procedures for water-soluble vitamins in foods and dietary supplements: a review. Anal Bioanal Chem. 2007;389:63-76. [DOI: 10.1007/s00216-007-1309-9].
7. Citová I, Havlíoková L, Urbánek L, Solichová D, Nováková l, Solich P. Comparison of a novel ultra-performance liquid chromatographic method for determination of retinol and α-tocoferol in human serum with conventional HPLC using monolithic and particulate columns. Anal Bioanal Chem. 2007;388(3):675-81. [DOI: 10.1007/s00216-007-1237-8].
8. Maldaner L, Jardim ICSF. O estado da arte da cromatografia líquida de ultra eficiência. Quím Nova. 2009;32(1):214-22. [DOI: 10.1590/S0100-40422009000100036].
9. Klimczak I, Gliszczyńska-Świglo A. Comparison of UPLC and HPLC methods for determination of vitamin C. Food Chem. 2015;175:100-5. [DOI:10.1016/j.foodchem.2014.11.104].
10. Pei Chen P, Wolf WR. LC/UV/MS-MRM for the simultaneous determination of water-soluble vitamins in multi-vitamin dietary supplements. Anal Bioanal Chem. 2007;387:2441-8. [DOI: 10.1007/s00216-006-0615-y].
11. Wilson N, Shah N.P. Review Paper: Microencapsulation of Vitamins. ASEAN Food Journal. 2007;14(1):1-14.
12. National Institute of Standards and Technology – NIST. Standard Reference Material. [acesso 2015 Out 08]. Disponível em: [https://www-s.nist.gov/srmors/view_detail.cfm?srm=3280].
13. Thomas JB, Sharpless KE, Yen JH, Rimmer CA. Determination of fat-soluble vitamins and carotenoids in standard reference material 3280 multivitamin/multielement tablets by liquid chromatography with absorbance detection. J AOAC Int. 2011;94(3):815-22.
14. Association of Oficial Analytical Chemists – AOAC. Official methods of analysis. 18th ed. Gaithersburg; 2005.
15. The United States Pharmacopeia – USP. 32nded. Rockville: The United States Pharmacopeial Convention; 2009.
16. Brasil. Ministério da Saúde. Resolução RDC nº 269, de 22 de setembro de 2005. Aprova o Regulamento Técnico sobre a Ingestão Diária Recomendada (IDR) de Proteína, Vitaminas e Minerais. Diário Oficial [da] República Federativa do Brasil. Brasília, DF, 23 set. 2005.
17. Instituto Nacional de Metrologia, Qualidade e Tecnologia – INMETRO. DOQ-CGCRE-008-Orientação sobre validação de métodos analíticos. Rev 04. Rio de Janeiro (RJ): Coordenação Geral de Acreditação; 2011.
18. Kand’ár R, Novotná P, Drábková P. Determination of retinol, α-tocopherol, lycopene, and β-carotene in human plasma using HPLC with UV-Vis detection: Application to a clinical study. J Chem. 2013; Article ID 460242, 7 p. [DOI: 10.1155/2013/460242].
19. Association of Oficial Analytical Chemists – AOAC. Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, 2002. [acesso 2015 Mar 02]. Disponível em: [http://www.aoac.org/imis15_prod/AOAC_Docs/StandardsDevelopment/SLV_Guidelines_Dietary_Supplements.pdf].
20. Brasil. Ministério da Saúde. Portaria nº 32, de 13 de janeiro de 1998. Aprova o regulamento técnico para fixação de identidade e qualidade de suplementos vitamínicos e ou de minerais. Diário Oficial [da] República Federativa do Brasil. Brasília, DF, 15 jan. 1998.
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