Analysis of Pharmacologic Adulteration in Dietary Supplements by Capillary Zone Electrophoresis Using Simultaneous Contactless Conductivity and UV Detection
The consumption of dietary supplements is increasing every year all over the world. In addition, the consumption has been accompanied by the increased frequency of adulteration of the products with synthetic pharmaceuticals. Analytical methods that allow testing the presence of synthetic drugs in dietary supplements are needed to detect such fraudulent practices. This paper describes the study of furosemide, hydrochlorothiazide, chlorthalidone and amiloride (diuretics), fluoxetine and paroxetine (antidepressants), and phenolphthalein (laxative) and amfepramone (anorexic) in dietary supplements marketed in Brazil for weight loss and physical fitness claims. A total of 113 products were acquired from websites and physical stores. The analytical method applied in this work involved the separation of the compounds by capillary zone electrophoresis in a working electrolyte consisting of 30% (v/v) methanol in a 20-mmol L−1 phosphate buffer (pH 9.2) and capacitively coupled contactless conductivity detection and UV detection simultaneously. The method was validated in accordance with the appropriate guideline of the Association of Analytical Communities (AOAC) and was successfully applied to the analysis of the samples of dietary supplements. Hydrochlorothiazide was present in 14 of the studied samples. One sample presented furosemide in addition to hydrochlorothiazide, both acting as diuretics.
KeywordsDietary supplements Adulterants Capillary electrophoresis Conductivity detection UV detection
The authors wish to acknowledge the financial support given by the Brazilian foundations CNPq, FAPERGS, and CAPES. The authors specially thank CAPES for the concession of a PDSE scholarship to L.S. Müller.
Compliance with Ethical Standards
This study was funded by CAPES, FAPERGS, and CNPq (Grant Numbers 440132/2014-2 and 312181/2013-2).
Conflict of interest
The authors declare that they have no conflict of interest.
This article does not contain any studies with human participants or animals performed by any of the authors.
- 4.Tainted products marketed as dietary supplements (2010) U.S. food and drug administration. http://www.fda.gov/ForConsumers/ConsumerUpdates/ucm236774.htm. Accessed 11 Apr 2017
- 14.Guo C, Shi F, Jiang S, Gong L, Zhao Y, Zhang J, Zeng S (2014) Simultaneous identification, confirmation and quantitation of illegal adulterated antidiabetics in herbal medicines and dietary supplements using high-resolution benchtop quadrupole-Orbitrap mass spectrometry. J Chromatogr B Biomed Sci Appl 967:174–182Google Scholar
- 15.Jiang S, Tan H, Guo C, Gong L, Shi F (2015) Development of an ultra-high-performance liquid chromatography coupled to high resolution quadrupole-Orbitrap mass spectrometry method for the rapid detection and confirmation of illegal adulterated sedative-hypnotics in dietary supplements. Food Addit Contam Part A Chem Anal Control Expo Risk Assess 32:1749–1759CrossRefGoogle Scholar
- 16.Shi F, Guo C, Gong L, Li J, Dong P, Zhang J, Cui P, Jiang S, Zhao Y, Zeng S (2014) Application of a high resolution benchtop quadrupole-Orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietary supplements. J Chromatogr A 1344:91–98CrossRefGoogle Scholar
- 20.Cianchino V, Acosta G, Ortega C, Martinez LD, Gomez MR (2008) Analysis of potential adulteration in herbal medicines and dietary supplements for the weight control by capillary electrophoresis. Anal Methods 108:1075–1081Google Scholar
- 31.AOAC (2013) Guidelines for dietary supplements and botanicals. Appendix K. AOAC Official Methods, RockvilleGoogle Scholar
- 32.Weiner IM, Goodman Gilman A, Rall TW, Nies AS, Taylor P (1990) Goodman and Gilman’s pharmacological basis of therapeutics. Pergamon, New YorkGoogle Scholar