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Current Pharmaceutical Analysis

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ISSN (Print): 1573-4129
ISSN (Online): 1875-676X

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Research Article

Simultaneous Analysis of Sexual Stimulants and Anabolic Steroids as Adulterants in Dietary Supplements by High Performance Liquid Chromatography with Photodiode Array Detection

Author(s): Carine Viana*, Gabriela Zanella Marcon, Thais Ramos Dal Molin, Denise Bohrer, Paulo Cícero do Nascimento and Leandro M. de Carvalho

Volume 17, Issue 6, 2021

Published on: 15 April, 2020

Page: [767 - 773] Pages: 7

DOI: 10.2174/1573412916999200415175325

Abstract

Background: The illegal virtual market for food supplements facilitates fraud and adulteration. Worldwide concern for consumer safety is growing on the part regulatory agencies, healthcare professionals and consumers.

Objective: This work aimed to evaluate the presence of sexual stimulants and anabolic steroids commonly used in the adulteration of dietary supplements through the development of a high performance liquid chromatography with the photodiode array detection (HPLC-DAD) method for the identification and quantification of these compounds.

Methods: The mobile phase composed of an ammonium acetate solution, acetonitrile and methanol led to the efficient separation of vardenafil, testosterone base, testosterone propionate, tadalafil, sildenafil and yohimbine.

Results: The assay was linear (r2> 0.999), precise (RSD% <0.5), accurate (99.1 to 105.2%), and the limits of detection and quantification were less than 0.05 and 0.15 μg/mL, respectively. Four samples of dietary supplements contained testosterone (n=1), tadalafil (n=2) and yohimbine (n=1) as adulterants. The adulterants found were in subtherapeutic doses, probably to reduce possible adverse effects and the action expected to appear natural. Since about 80% of adverse drug reactions are dose dependent, unpredictable adverse drug reactions are dose independent and based on idiosyncratic or allergic mechanisms or intolerance. Conclusion: The developed method is convenient and easily applicable for adulteration detection of the analyzed drugs in the multicomponent supplements.

Keywords: Adulterants, anabolic steroids, dietary supplements, liquid chromatography with photodiode array, sexual stimulants, dysfunction.

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Graphical Abstract

[1]
Müller, L.S.; Dal Molin, T.R.; Muratt, D.T.; Leal, G.C.; Urquhart, C.G.; Viana, C.; Carvalho, L.M. Determination of Stimulants and Diuretics in Dietary Supplements for Weight Loss and Physical Fitness by Ion-pair Chromatography and Pulsed Amperometric Detection (PAD). Curr. Anal. Chem., 2018, 14, 562-570.
[http://dx.doi.org/10.2174/1573411014666171229155726]
[2]
Molin, T.R.D.; Leal, G.C.; Müller, L.S.; Muratt, D.T.; Marcon, G.Z.; Carvalho, L.M.; Viana, C. Regulatory framework for dietary supplements and the public health challenge. Rev. Saude Publica, 2019, 53, 90.
[http://dx.doi.org/10.11606/s1518-8787.2019053001263] [PMID: 31644771]
[3]
Brazil. Agência Nacional de Vigilância Sanitária. RDC nº 243, de 26 de julho de 2018. Dispõe sobre os requisitos sanitários dos suplementos alimentares. Diário Oficial União, 2018, 1, 100.. 2018.http://portal.anvisa.gov.br/documents/10181/2718376/RDC_18_2010_COMP.pdf/1f6e1baf-fd83-4408-8e97-07578fe3db18 (Accessed January 29, 2020).
[4]
Viana, C.; Zemolin, G.M.; Dal Molin, T.R.; Gobo, L.; Ribeiro, S.M.; Leal, G.C.; Marcon, G.Z.; de Carvalho, L.M. Detection and determination of undeclared synthetic caffeine in weight loss formulations using HPLC-DAD and UHPLC-MS/MS. J. Pharm. Anal., 2018, 8(6), 366-372.
[http://dx.doi.org/10.1016/j.jpha.2017.12.004] [PMID: 30595942]
[5]
Viana, C.; Zemolin, G.M.; Müller, L.S.; Dal Molin, T.R.; Seiffert, H.; de 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. Part A Chem. Anal. Control Expo. Risk Assess., 2016, 33(1), 1-9.
[PMID: 26560757]
[6]
Parra, R.M.T.; Palma, A.; Pierucci, A.P.T.R. Contaminação de suplementos dietéticos usados para prática esportiva: uma revisão de literatura. Rev. Bras. Ciênc. Esporte, 2011, 33, 1071-1084.
[http://dx.doi.org/10.1590/S0101-32892011000400018]
[7]
Patel, D.N.; Li, L.; Kee, C.L.; Ge, X.; Low, M.Y.; Koh, H.L. Screening of synthetic PDE-5 inhibitors and their analogues as adulterants: analytical techniques and challenges. J. Pharm. Biomed. Anal., 2014, 87, 176-190.
[http://dx.doi.org/10.1016/j.jpba.2013.04.037] [PMID: 23721687]
[8]
Zou, P.; Oh, S.S.; Hou, P.; Low, M.Y.; Koh, H.L. Simultaneous determination of synthetic phosphodiesterase-5 inhibitors found in a dietary supplement and pre-mixed bulk powders for dietary supplements using high-performance liquid chromatography with diode array detection and liquid chromatography-electrospray ionization tandem mass spectrometry. J. Chromatogr. A, 2006, 1104(1-2), 113-122.
[http://dx.doi.org/10.1016/j.chroma.2005.11.103] [PMID: 16364350]
[9]
Sun, J.; Chen, P. Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS. J. Pharm. Biomed. Anal., 2012, 61, 142-149.
[http://dx.doi.org/10.1016/j.jpba.2011.11.013] [PMID: 22221902]
[10]
Christou, M.A.; Christou, P.A.; Markozannes, G.; Tsatsoulis, A.; Mastorakos, G.; Tigas, S. Effects of Anabolic Androgenic Steroids on the Reproductive System of Athletes and Recreational Users: A Systematic Review and Meta-Analysis. Sports Med., 2017, 47(9), 1869-1883.
[http://dx.doi.org/10.1007/s40279-017-0709-z] [PMID: 28258581]
[11]
Hackney, A.C. Doping, Performance-Enhancing Drugs, and Hormones in Sport: Mechanisms of Action and Methods of Detection; Elsevier, 2017.
[12]
El Osta, R.; Almont, T.; Diligent, C.; Hubert, N.; Eschwège, P.; Hubert, J. Anabolic steroids abuse and male infertility. Basic Clin. Androl., 2016, 26, 2.
[PMID: 26855782]
[13]
Gilard, V.; Balayssac, S.; Tinaugus, A.; Martins, N.; Martino, R.; Malet-Martino, M. Detection, identification and quantification by 1H NMR of adulterants in 150 herbal dietary supplements marketed for improving sexual performance. J. Pharm. Biomed. Anal., 2015, 102, 476-493.
[http://dx.doi.org/10.1016/j.jpba.2014.10.011] [PMID: 25459948]
[14]
Harris, D.C.; Lucy, C. Quantitative Chemical Analysis; W. H. Freeman: New York, 2012.
[15]
Association of Official Analytical Chemists. AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, 2013.http://members.aoac.org/aoac_prod_imis/AOAC_Docs/StandardsDevelopment/SLV_Guidelines_Dietary_Supplements.pdf
[16]
The United States Pharmacopeia (USP). U.S. Pharmacopeia 40/National Formulary 35, The United States Pharmacopeial Convention, Inc. Rockville, . 2017.
[17]
Geyer, H.; Parr, M.K.; Mareck, U.; Reinhart, U.; Schrader, Y.; Schänzer, W. Analysis of non-hormonal nutritional supplements for anabolic-androgenic steroids - results of an international study. Int. J. Sports Med., 2004, 25(2), 124-129.
[http://dx.doi.org/10.1055/s-2004-819955] [PMID: 14986195]
[18]
Petróczi, A.; Taylor, G.; Naughton, D.P. Mission impossible? Regulatory and enforcement issues to ensure safety of dietary supplements. Food Chem. Toxicol., 2011, 49(2), 393-402.
[http://dx.doi.org/10.1016/j.fct.2010.11.014] [PMID: 21087651]
[19]
Damiano, F.; Silva, C.; Gregori, A.; Vacondio, F.; Mor, M.; Menozzi, M.; Di Giorgio, D. Analysis of illicit dietary supplements sold in the Italian market: identification of a sildenafil thioderivative as adulterant using UPLC-TOF/MS and GC/MS. Sci. Justice, 2014, 54(3), 228-237.
[http://dx.doi.org/10.1016/j.scijus.2014.02.009] [PMID: 24796952]
[20]
Fonseca, H.P.; Scapinelli, A.; Aoki, T.; Aldrighi, J. Deficiência androgênica na mulher. Rev. Assoc. Med. Bras., 2010, 56, 579-582.
[http://dx.doi.org/10.1590/S0104-42302010000500021] [PMID: 21152832]
[21]
Gong, B.; Ma, M.; Xie, W.; Yang, X.; Huang, Y.; Sun, T.; Luo, Y.; Huang, J. Direct comparison of tadalafil with sildenafil for the treatment of erectile dysfunction: a systematic review and meta-analysis. Int. Urol. Nephrol., 2017, 49(10), 1731-1740.
[http://dx.doi.org/10.1007/s11255-017-1644-5] [PMID: 28741090]
[22]
Zhang, Y.; Huang, Z.; Ding, L.; Yan, H.; Wang, M.; Zhu, S. Simultaneous determination of yohimbine, sildenafil, vardenafil and tadalafil in dietary supplements using high-performance liquid chromatography-tandem mass spectrometry. J. Sep. Sci., 2010, 33(14), 2109-2114.
[http://dx.doi.org/10.1002/jssc.200900841] [PMID: 20533336]
[23]
Kant, A.; Bilmen, J.; Hopkins, P.M. Adverse Drug Reactions., 2019.
[24]
Gurzu, S.; Jung, I. Textbook of Iatrogenic Pathology; Bentham Science Publishers, 2017.
[http://dx.doi.org/10.2174/97816810851421170101]

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