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Current Analytical Chemistry

Editor-in-Chief

ISSN (Print): 1573-4110
ISSN (Online): 1875-6727

Research Article

Quantification of Alpha Lipoic Acid in Pharmaceutical Products by HPLC with Pulsed Amperometric Detection at a Gold Electrode

Author(s): Carine Viana*, Sandra M. Ribeiro, Ana P.L. Moreira, Larissa S. Müller, Monique J. Motta, José M. Monserrat, Leandro M. de Carvalho and Denise Bohrer

Volume 15, Issue 6, 2019

Page: [694 - 700] Pages: 7

DOI: 10.2174/1573411014666180418155615

Price: $65

Abstract

Background: Alpha-lipoic acid (ALA) has become a common ingredient in food supplements and multivitamin formulas. ALA is widely used as therapy for preventing diabetic polyneuropathies, scavenges free radicals, and restores intracellular glutathione levels. This study aimed to develop a simple and fast analytical method to determine ALA content in dietary supplements using highperformance liquid chromatography with pulsed amperometric detection (HPLC PAD).

Methods: ALA was analyzed by HPLC in a mobile phase composed of 25 mmol/L potassium phosphate in 50% (v/v) acetonitrile (pH 4.0) and PAD at a gold electrode (vs. solid-phase hydrogen reference electrode). The PAD cycle was performed by applying a detection potential (E1) of +0.7 V for 0.4 s, an oxidation potential (E2) of +1.0V for 0.4 s and a reduction potential (E3) of -0.2 V for 1.2 s.

Results: The runtime method was shown a rapid procedure for the analysis of α-lipoic acid. The sampling rate of 8 injections per hour was attained and measurements of the reproducibility of successive injections (20 µL) showed an RSD of 1.89% for 16 successive injections. The method presented low quantification limit of 0.21 mg/L. The industrialized ALA-based supplements ranged from to 97.8 to 104.1%, while manipulated capsules ranged from 69.2 to 95.4%.

Conclusion: Electrochemical detector has been presented as an effective alternative for ALA determination, which has weakly UV-absorbing. This detection has the benefits of sensitivity, simplicity and low costs. The developed HPLC-DAD method proposes to be analytical tool applicable to quality control of ALA supplements.

Keywords: Alpha lipoic acid, Food supplements, HPLC, Pulsed amperometric detection, Gold electrode, Electrochemical detector.

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[1]
Durrani, A.I.; Schwartz, H.; Nagi, M.; Sontag, G. Determination of free α-lipoic acid in foodstuffs by HPLC coupled with CEAD and ESI-MS. Food Chem., 2010, 120, 1143-1148.
[2]
Siangproh, W.; Rattanarat, P.; Chailapakul, O. Reverse-phase liquid chromatographic determination of α-lipoic acid in dietary supplements using a boron-doped diamond electrode. J. Chrom. A., 2010, 1217, 7699-7705.
[3]
Navari-Izzo, F.; Quartacci, M.F.; Sgherri, C. Lipoic acid: A unique antioxidant in the detoxification of activated oxygen species. Plant Physiol. Biochem., 2002, 40, 463-470.
[4]
Foster, T.S. Efficacy and safety of a-lipoic acid supplementation in the treatment of symptomatic diabetic neuropathy. Diabet Educator., 2007, 33, 111-117.
[5]
Kizhakekuttu, T.J.; Widiansky, M. Natural antioxidants and hypertension: Promise and challenges. Cardiovasc. Ther., 2010, 28, 20-32.
[6]
Hah, Y.S.; Sung, M.J.; Lim, H.S.; Jun, J.S.; Jeong, Y.G.; Kim, H.O.; Kim, J.; Hur, H.J.; Devaatseren, M.; Know, D.Y.; Lee, S.I. Dietary alpha lipoic acid supplementation prevents synovial in examination and bone destruction in collagen-induced arthritic mice. Rheumatol. Int., 2011, 31, 1583-1590.
[7]
Khabbazi, T.; Mahdavi, R.; Safa, J.; Pour-Abdollahi, P. Effects of alpha-lipoic acid supplementation on inflammation, oxidative stress, and serum lipid profile levels in patients with end-stage renal disease on hemodialysis. J. Renal. Nutr., 2012, 22, 244-250.
[8]
Miranda, M.P.; Del Rio, R.; Del Valle, M.A.; Faundez, M.; Armijo, F. Use of fluorine-doped tin oxide electrodes for lipoic acid determination in dietary supplements. J. Electroanal. Chem., 2012, 668, 1-6.
[9]
Durrani, A.I.; Schwartz, H.; Schmid, W.; Sontag, G. α-Lipoic acid in dietary supplements: Development and comparison of HPLC-CEAD and HPLC ESI-MS methods. J. Pharm. Biom. Anal., 2007, 45, 694-699.
[10]
Sitton, A.; Schmid, M.G.; Gübitz, G.; Aboul-Enein, H.Y. Determination of lipoic acid in dietary supplement preparations by capillary electrophoresis. J. Biochem. Biophys. Meth, 2004, 61, 119-124.
[11]
Vani, R.; Vijaya Kumar, B.; Krishna Mohan, G. Analytical method development and validation for the determination of allopurinol and alphalipoic acid using reverse phase HPLC method in bulk and tablet dosage form. Res. J. Pharm. Tech, 2015, 8, 207-211.
[12]
Aboul-Enein, H.Y.; Hoenen, H. Validated method for determination of α-lipoic acid in dietary supplement tablets by reversed phase liquid chromatography. J. Liq. Chrom. Rel. Technol., 2004, 27, 3029-3038.
[13]
Sitton, A.; Schmid, M.G.; Gübitz, G.; Aboul-Enein, H.Y. Determination of lipoic acid in dietary supplement preparations by capillary electrophoresis. J. Biochem. Biophys. Meth, 2004, 61, 119-124.
[14]
Khan, A.; Khan, M.I.; Iqbal, Z.; Ahmad, L.; Shah, Y.; Watson, D.G. Determination of lipoic acid in human plasma by HPLC-ECD using liquid–liquid and solid-phase extraction: Method development, validation and optimization of experimental parameters. J. Chrom. B., 2010, 878, 2782-2788.
[15]
Khan, A.; Iqbal, Z.; Watson, D.G.; Khan, A.; Khan, I.; Muhammad, N.; Muhammad, S.; Nasib, H.A.; Iqbal, N. Faiz-Ur-Rehman; Kashif, M. Simultaneous determination of lipoic acid (LA) and dihydrolipoic acid (DHLA) in human plasma using high-performance liquid chromatography coupled with electrochemical detection. J. Chrom. B., 2011, 879, 1725-1731.
[16]
Teichert, J.; Preiss, R. High-performance liquid chromatographic assay for α-lipoic acid and five of its metabolites in human plasma and urine. J. Chrom. B., 2002, 769, 269-281.
[17]
Official Methods of Analytical Chemists of AOAC International, 15th; Ed. Washington, DC, USA, Association of Official Analytical Chemists, 1990.
[18]
Lacourse, W.R.; Dasenbrock, C.O. Pulsed electrochemical detection of sulfur-containing antibiotics following high performance liquid chromatography. J. Pharmac. Biom. Anal, 1999, 19, 239-252.
[19]
Lacourse, W.R.; Owens, G.S. Pulsed electrochemical detection of thiocompounds following microchromatographic separations. Anal. Chim. Acta, 1995, 307, 301-319.
[20]
Lee, J.W.; Yeo, I.H. Integrated pulsed amperometry for the analysis of organic compounds. Microchem. J., 2001, 70, 173-177.
[21]
Viana, C.; Zemolin, G.M.; Müller, L.S.; Dal Molin, T.R.; Seiffert, H.; Carvalho, L.M. Liquid chromatographic determination of caffeine and adrenergic stimulants in food supplements sold in Brazilian e-commerce for weight loss and physical fitness. Food Addit. Contam. A, 2016, 33, 1-9.
[22]
Brazil. Ministério da Saúde. Anvisa. Resolução da Diretoria Colegiada (RDC) no 16. Aprova o Regulamento Técnico de Procedimentos para registro de Alimentos e ou Novos Ingredientes. (1999a). http://pesquisa.in.gov.br/imprensa/jsp/visualiza/index.jsp?data=03/05/1999&jornal=1&pagina=11&totalArquivos=111 (Accessed Dec 13, 2017)
[23]
Brazil. Ministério da Saúde. Anvisa. RDC no 17. Regulamento Técnico que estabelece as Diretrizes Básicas para a Avaliação de Risco e Segurança dos Alimentos. (1999b) http://pesquisa. in.gov.br/imprensa/jsp/visualiza/index.jsp?data=03/05/1999&jornal=1&pagina=11&totalArquivos=111 (Accessed Dec 13, 2017)
[24]
Brazil. Ministério da Saúde. Anvisa. RDC no 28. Regulamento Técnico de Bens e Produtos Importados para fins de Vigilância Sanitária (2011). http://bvsms.saude.gov.br/bvs/saudelegis/anvisa/ 2011/res0028_28_06_2011.html (Accessed Dec 13, 2017)
[25]
Brazil. Ministério da Saúde. Anvisa. RDC no 67. Boas Práticas de Manipulação de Preparações Magistrais e Oficinais para Uso Humano em farmácias (2007). http://pesquisa.in.gov.br/imprensa/ jsp/visualiza/index.jsp?jornal=1&pagina=29&data=09/10/2007 (Accessed Dec 13, 2017)
[26]
United States Government Accountability Office (U.S. GAO), Drug Compounding. FDA Has Taken Steps to Implement Compounding Law, but Some States and Stakeholders Reported Challenges, Report to Congressional Committees GAO-17-64, 2016. http://www.gao.gov/products/GAO-17-64 (Accessed Dec 13, 2017)
[27]
US Food and Drug Administration (FDA). Pharmacy Compounding of Human Drug Products Under Section 503A of the Federal Food, Drug, and Cosmetic Act: Guidance, June 9, 2016 https://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/UCM469119.pdf (Accessed Dec 13, 2017)

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