An Analysis for Adulteration and Contamination of Over-the-Counter Weight-Loss Products


Six Australian and five overseas complementary medicines (CM) and meal replacement shake products were analysed for potential adulteration with two common active pharmaceutical ingredients, caffeine and sibutramine, using thin-layer chromatography and mass spectrometry. The declared amount of caffeine in each product was also reviewed. Finally, the products were examined for heavy metal contamination using inductively coupled plasma-mass spectrometry. The results showed that there was no detected adulteration of either caffeine (for those products that did not list caffeine as an ingredient) or sibutramine in the 11 products; however, based on the product labels, one Australian and one overseas (two in total) CM product contained more than the maximum daily safety limit (400 mg) of caffeine. Potentially excessive lead and/or chromium was detected in six products, including four Australian products and two products purchased online. One Australian CM product appeared to contain these heavy metals at concentrations at, or exceeding, the safety limits specified in the United States Pharmacopeia or set by the World Health Organization. The overconsumption of caffeine and heavy metals has the potential of causing significant health effects in consumers.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2


  1. 1.

    Wright KL, Verney K, Brennan D, Lindsay D, Lindsay D, Smyth W. Administrative staff-self reported long-term conditions: findings from a regional Australian health service. Int J Workplace Health Manag. 2019;12(6):483–94.

    Article  Google Scholar 

  2. 2.

    Ee C, Cave AE, Naidoo D, Boyages J. Prevalence of and attitudes towards complementary therapy use for weight after breast cancer in Australia: a national survey. BMC Complement Altern Med. 2019;19(1):1–10.

    Article  CAS  Google Scholar 

  3. 3.

    Yoong SL, Carey ML, Sanson-Fisher RW, D’Este C. A cross-sectional study assessing the self-reported weight loss strategies used by adult Australian general practice patients. BMC Fam Pract. 2012;13(1):48.

    PubMed  PubMed Central  Article  Google Scholar 

  4. 4.

    Lauche R, Fuller NR, Cramer H, Wardle J, Sibbritt D, Adams J. Associations between complementary medicine, satisfaction with body weight and shape, and the use of methods to lose or control weight: results of a national survey of 8009 Australian women. Complement Ther Med. 2018;36:100–6.

    PubMed  Article  Google Scholar 

  5. 5.

    Harvey K. Regulation of complementary medicines. Intern Med J. 2017;47(9):983–5.

    PubMed  Article  Google Scholar 

  6. 6.

    Müller LS, Moreira APL, Muratt DT, Viana C, De Carvalho LM. An ultra-high performance liquid chromatography–electrospray tandem mass spectrometric method for screening and simultaneous determination of anorexic, anxiolytic, antidepressant, diuretic, laxative and stimulant drugs in dietary supplements marketed for weight loss. J Chromatogr Sci. 2019;57(6):528–40.

    PubMed  Article  CAS  Google Scholar 

  7. 7.

    Hachem R, Assemat G, Martins N, Balayssac S, Gilard V, Martino R, et al. Proton NMR for detection, identification and quantification of adulterants in 160 herbal food supplements marketed for weight loss. J Pharm Biomed Anal. 2016;124:34–47.

    CAS  PubMed  Article  Google Scholar 

  8. 8.

    Taing MW, Tan ETX, Williams GM, Clavarino AM, McGuire TM. Herbal and nutrient complementary medicines for weight loss: community pharmacists’ practices, attitudes, recommendations, information and education needs. Int J Pharm Pract. 2016;24(3):160–9.

    PubMed  Article  Google Scholar 

  9. 9.

    Mathon C, Ankli A, Reich E, Bieri S, Christen P. Screening and determination of sibutramine in adulterated herbal slimming supplements by HPTLC-UV densitometry. Food Addit Contam Part A. 2014;31(1):15–20.

    CAS  Article  Google Scholar 

  10. 10.

    Khazan M, Hedayati M, Kobarfard F, Askari S, Azizi F. Identification and determination of synthetic pharmaceuticals as adulterants in eight common herbal weight loss supplements. Iran Red Crescent Med J. 2014;16(3):e15344.

    PubMed  PubMed Central  Article  Google Scholar 

  11. 11.

    Doménech-Carbóa A, Martinib M, de Carvalhob LM, Vianab C, Doménech-Carbóc MT, Silva M. Screening of pharmacologic adulterant classes in herbal formulations using voltammetry of microparticles. J Pharm Biomed Anal. 2013;74:194–204.

    Article  CAS  Google Scholar 

  12. 12.

    Trigueros L, Peña S, Ugidos A, Sayas-Barberá E, Pérez-Álvarez J, Sendra E. Food ingredients as anti-obesity agents: a review. Crit Rev Food Sci Nutr. 2013;53(9):929–42.

    CAS  PubMed  Article  Google Scholar 

  13. 13.

    Tallett A, Blundell J, Rodgers R. Sibutramine & naloxone: infra-additive interaction in the regulation of appetite? Behav Brain Res. 2010;207(1):174–81.

    CAS  PubMed  Article  Google Scholar 

  14. 14.

    James WPT, Caterson ID, Coutinho W, Finer N, Van Gaal LF, Maggioni AP, et al. Effect of sibutramine on cardiovascular outcomes in overweight and obese subjects. N Engl J Med. 2010;363(10):905–17.

    CAS  PubMed  Article  Google Scholar 

  15. 15.

    Gurley BJ, Steelman SC, Thomas SL. Multi-ingredient, caffeine-containing dietary supplements: history, safety, and efficacy. Clin Ther. 2015;37(2):275–301.

    CAS  PubMed  Article  Google Scholar 

  16. 16.

    Viana C, Zemolin GM, Dal Molin TR, Gobo L, Ribeiro SM, Leal GC, et al. Detection and determination of undeclared synthetic caffeine in weight loss formulations using HPLC-DAD and UHPLC-MS/MS. J Pharm Anal. 2018;8(6):366–72.

    PubMed  Article  Google Scholar 

  17. 17.

    Musgrave IF, Farrington RL, Hoban C, Byard RW. Caffeine toxicity in forensic practice: possible effects and under-appreciated sources. Forensic Sci Med Pathol. 2016;12(3):299–303.

    CAS  PubMed  Article  Google Scholar 

  18. 18.

    Bessada SM, Alves RC, Oliveira MBP. Caffeine-based food supplements and beverages: trends of consumption for performance purposes and safety concerns. Food Res Int. 2018;109:310–9.

    CAS  PubMed  Article  Google Scholar 

  19. 19.

    Neves DBDJ, Caldas ED. Determination of caffeine and identification of undeclared substances in dietary supplements and caffeine dietary exposure assessment. Food Chem Toxicol. 2017;105:194–202.

    CAS  PubMed  Article  Google Scholar 

  20. 20.

    Pascali JP, Fais P, Vaiano F, Bertol E. Application of 404 HRAM screening and LC–MS/MS confirmation of active pharmaceutical ingredient in “natural” herbal supplements. Forensic Sci Int. 2018;286:e28–31.

    CAS  PubMed  Article  Google Scholar 

  21. 21.

    Hoban CL, Musgrave IF, Coghlan ML, Power MW, Byard RW, Nash C, et al. Adulterants and contaminants in psychotropic herbal medicines detected with mass spectrometry and next409 generation DNA sequencing. Pharm Med. 2018;32(6):429–44.

    CAS  Article  Google Scholar 

  22. 22.

    Bolan S, Kunhikrishnan A, Seshadri B, Choppala G, Naidu R, Bolan NS, et al. Sources, distribution, bioavailability, toxicity, and risk assessment of heavy metal(loid)s in complementary medicines. Environ Int. 2017;108:103–18.

    CAS  PubMed  Article  Google Scholar 

  23. 23.

    Flegal AR, Gallon C, Ganguli PM, Conaway CH. All the lead in China. Crit Rev Environ Sci Technol. 2013;43(17):1869–944.

    CAS  Article  Google Scholar 

  24. 24.

    Breeher L, Gerr F, Fuortes L. A case report of adult lead toxicity following use of Ayurvedic herbal medication. J Occup Med Toxicol. 2013;8(1):26.

    PubMed  PubMed Central  Article  Google Scholar 

  25. 25.

    Lin H, Chou S, Yang H, Hwang Y, Kuo C, Kao T, et al. Association of blood lead and mercury with estimated GFR in herbalists after the ban of herbs containing aristolochic acids in Taiwan. Occup Environ Med. 2013;70(8):545–51.

    CAS  PubMed  Article  Google Scholar 

  26. 26.

    Filippini M, Baldisserotto A, Menotta S, Fedrizzi G, Rubini S, Gigliotti D, et al. Heavy metals and potential risks in edible seaweed on the market in Italy. Chemosphere. 2020;263:127983.

    PubMed  Article  CAS  Google Scholar 

  27. 27.

    Gao Y, Li X, Dong J, Cao Y, Li T, Mielke HW. Snack foods and lead ingestion risks for school aged children: a comparative evaluation of potentially toxic metals and children’s exposure response of blood lead, copper and zinc levels. Chemosphere. 2020;261:127547.

    CAS  PubMed  Article  Google Scholar 

  28. 28.

    Korfali SI, Hawi T, Mroueh M. Evaluation of heavy metals content in dietary supplements in Lebanon. Chem Cent J. 2013;7(1):10.

    CAS  PubMed  PubMed Central  Article  Google Scholar 

  29. 29.

    Abdulla NM, Adam B, Blair I, Oulhaj A. Heavy metal content of herbal health supplement products in Dubai–UAE: a cross-sectional study. BMC Complement Altern Med. 2019;19(1):276.

    PubMed  PubMed Central  Article  CAS  Google Scholar 

  30. 30.

    Sundar S, Chakravarty J. Antimony toxicity. Int J Environ Res Public Health. 2010;7(12):4267–77.

    CAS  PubMed  PubMed Central  Article  Google Scholar 

  31. 31.

    Sun H, Brocato J, Costa M. Oral chromium exposure and toxicity. Curr Environ Health Rep. 2015;2(3):295–303.

    CAS  PubMed  PubMed Central  Article  Google Scholar 

  32. 32.

    Shekhawat K, Chatterjee S, Joshi B. Chromium toxicity and its health hazards. Int J Adv Res. 2015;3(7):167–72.

    CAS  Google Scholar 

  33. 33.

    Csupor D, Boros K, Dankó B, Veres K, Szendrei K, Hohmann J. Rapid identification of sibutramine in dietary supplements using a stepwise approach. Die Pharmazie. 2013;68(1):15–8.

    CAS  PubMed  Google Scholar 

  34. 34.

    Petkova-Gueorguieva E, Ivanov K, Gueorguiev S, Mihaylova A, Madzharov V, Ivanova S. Detection of sibutramine in herbal food supplements by UHPLC/HRMS and UHPLC/MS-MS. Biomed Res. 2018;29(14):3006–9.

    CAS  Google Scholar 

  35. 35.

    Gray LJ, Cooper N, Dunkley A, Warren FC, Ara R, Abrams K, et al. A systematic review and mixed treatment comparison of pharmacological interventions for the treatment of obesity. Obes Rev. 2012;13(6):483–98.

    CAS  PubMed  Article  Google Scholar 

  36. 36.

    Muschietti L, Redko F, Ulloa J. Adulteration of selected dietary supplements and their detection methods. Drug Test Anal. 2020;12(7):861–86.

    CAS  PubMed  Article  Google Scholar 

  37. 37.

    Gu X, Jin Y, Dong F, Cai Y, You Z, You J, et al. Toward rapid analysis, forecast and discovery of bioactive compounds from herbs by jointly using thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy technique. J Pharm Biomed Anal. 2018;153:9–15.

    CAS  PubMed  Article  Google Scholar 

  38. 38.

    Phattanawasin P, Sotanaphun U, Sukwattanasinit T, Akkarawaranthorn J, Kitchaiya S. Quantitative determination of sibutramine in adulterated herbal slimming formulations by TLC image analysis method. Forensic Sci Int. 2012;219(1-3):96–100.

    CAS  PubMed  Article  Google Scholar 

  39. 39.

    Therapeutic Goods Administration. High-moderate risk changes to permissible ingredients - Caffeine 2019 [Available from: ingredients-caffeine.

  40. 40.

    Food Standards Australia New Zealand. Caffeine 2019 [Available from:

  41. 41.

    British Pharmacopeia Commission. British Pharmacopoeia 2020 (Ph. Eur. 10.2). London2020.

  42. 42.

    Vincent JB. New evidence against chromium as an essential trace element. J Nutr. 2017;147(12):2212–9.

    CAS  PubMed  Article  Google Scholar 

  43. 43.

    Milačič R, Ščančar J. Cr speciation in foodstuffs, biological 462 and environmental samples: methodological approaches and analytical challenges–a critical review. Trends Anal Chem. 2020;127:115888.

    Article  CAS  Google Scholar 

  44. 44.

    United States Pharmacopeia Convention. USP43-NF38. General Chapter <2232> Elemental Contaminants In Dietary Supplements. Rockville (MD)2020.

  45. 45.

    Bishop DP, Hare DJ, Clases D, Doble PA. Applications of liquid chromatography-inductively coupled plasma-mass spectrometry in the biosciences: a tutorial review and recent developments. Trends Anal Chem. 2018;104:11–21.

    CAS  Article  Google Scholar 

Download references

Author information



Corresponding author

Correspondence to Nial J. Wheate.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Wong, P.H.B., Harnett, J.E., Clases, D. et al. An Analysis for Adulteration and Contamination of Over-the-Counter Weight-Loss Products. AAPS PharmSciTech 22, 78 (2021).

Download citation

Key Words

  • adulteration
  • heavy metal
  • contamination
  • complementary medicine
  • patient safety