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Application of HPLC for detection of sildenafil/tadalafil in marketed honey in Oman

Year 2025, Volume: 12 Issue: 2, 297 - 305

Abstract

Honey adulteration allegedly with phosphodiesterase-5 (PDE-5) inhibitors including sildenafil, and tadalafil is a common and dangerous practice. This study aimed to develop a procedure to detect the presence of common adulterants namely sildenafil and tadalafil using RP-HPLC. Seven commercial honey samples of local and international origin were collected from supermarkets and honey sellers. Both the adulterants in honey samples were identified and quantified with the help of an HPLC technique. Chromatographic separation was done in RP-HPLC mode using buffer: methanol: acetonitrile (5.8: 2.5: 1.7) mobile phase and diode array as a detector. The buffer used was 0.05 M Triethylamine orthophosphate pH (3.0). The results showed that four honey samples (HAD1, HAD5, HAD6, and HAD7) were adulterated with sildenafil, and among them, HAD5 contained the maximum amount of sildenafil as 22.65 mg/g of the honey sample. However, only 2 honey samples HAD4 and HAD6 were found to be adulterated with tadalafil (1.248 and 0.7 mg/g) of the tested honey sample. The result of this study warrants rigorous quality control of the commercially available honey products in Oman by the authorities. The consumption of adulterated honey samples may impact the health of consumers hence further detailed studies must be carried out to confirm the findings of the current study and novel analytical methods be developed to detect the level of other possible adulterants in this valuable product.

Ethical Statement

EBS/PRES0401-COP/04/2022-23 College of Pharmacy, National University of Science and Technology, Azaiba, Muscat, Sultanate of Oman.

Supporting Institution

MoH Sultanate of Oman

Project Number

EBS/PRES0401-COP/04/2022-23

References

  • Abdelshakour, M.A., Salam, R.A.A., Hadad, G.M., Abo-ElMatty, D.M., & Hameed, E.A. A. (2021). HPLC-UV and UPLC-MS/MS methods for the simultaneous analysis of sildenafil, vardenafil, and tadalafil and their counterfeits dapoxetine, paroxetine, citalopram, tramadol, and yohimbine in aphrodisiac products. RSC advances, 11(14), 8055-8064. https://doi.org/10.1039/d0ra10324a
  • Agency, E.M. (1995). ICH Topic Q 2 (R1) validation of analytical procedures: text and methodology. Prescrire International, 20, 278.
  • Al Lawati, H.A., Al Busaidi, I., Kadavilpparampu, A.M., & Suliman, F.O. (2017). Determination of common adulterants in herbal medicine and food samples using core-shell column coupled to tandem mass spectrometry. Journal of Chromatographic Science, 55(3), 232-242. https://10.1093/chromsci/bmw175
  • Ala'Y, S., AlRashdan, Y., Abbasi, N.U., Mostafa, A., Abudayeh, Z., Talhouni, A., & Al-Ebini, Y. (2023). Optimization and validation of HPLC-UV method for the determination of vardenafil, sildenafil, and tadalafil in honey-mixed herbal sachets using a design of experiment. Jordan Journal of Pharmaceutical Sciences, 16(1), 148 162. https://10.35516/jjps.v16i1.1075
  • Bogusz, M.J., Hassan, H., Al-Enazi, E., Ibrahim, Z., & Al-Tufail, M. (2006). Application of LC–ESI–MS–MS for detection of synthetic adulterants in herbal remedies. Journal of Pharmaceutical and Biomedical Analysis, 41(2), 554 564. https://doi.org/10.1016/j.jpba.2005.12.015
  • Cárdenas-Escudero, J., Galán-Madruga, D., & Cáceres, J. (2023). FTIR-ATR detection method for emerging C3-plants-derivated adulterants in honey: Beet, dates, and carob syrups. Talanta, 124768. https://doi.org/10.1016/j.talanta.2023.124768
  • Dou, X., Zhang, L., Chen, Z., Wang, X., Ma, F., Yu, L., ... Li, P. (2023). Establishment and evaluation of multiple adulteration detection of camellia oil by mixture design. Food Chemistry, 406, 135050. https://doi.org/10.1016/j.foodchem.2022.135050
  • Fakhlaei, R., Selamat, J., Khatib, A., Razis, A. F. A., Sukor, R., Ahmad, S., & Babadi, A. A. (2020). The toxic impact of honey adulteration: A review. Foods, 9(11), 1538. https://10.3390/foods9111538
  • FDA. (2022). FDA Warns Four Companies for Selling Tainted Honey-based Products with Hidden Active Drug Ingredients. FDA News Release. https://www.prnewswire.com/news-releases/fda-warns-four-companies-for-selling-tainted-honey-based-products-with-hidden-active-drug-ingredients-301584930.html
  • Gong, B., Ma, M., Xie, W., Yang, X., Huang, Y., Sun, T., ... Huang, J. (2017). Direct comparison of tadalafil with sildenafil for the treatment of erectile dysfunction: a systematic review and meta-analysis. International Urology and Nephrology, 49, 1731-1740. https://doi.org/10.1007/s11255-017-1644-5
  • González-Ceballos, L., Guirado-Moreno, J.C., Utzeri, G., García, J.M., Fernández-Muino, M.A., Osés, S.M., ... Vallejos, S. (2023). Straightforward purification method for the determination of the activity of glucose oxidase and catalase in honey by extracting polyphenols with a film-shaped polymer. Food Chemistry, 405, 134789. https://doi.org/10.1016/j.foodchem.2022.134789
  • Mehryar, L., & Esmaiili, M. (2011). Honey & honey adulteration detection: A review. Proceedings of 11th International Congress on Engineering and Food, NFP1066-libre.pdf
  • Ng, C.M., & Reuter, W.M. (2015). Analysis of Sugars in Honey Using the PerkinElmer Altus HPLC System with RI Detection. Perkin Elmer, Inc, 1 5. https://www.slideshare.net/perkinelmerinc/analysis-of-sugars-in-honey-using-the-perkinelmer-altus-hplc-system-with-ri-detection
  • Pannu, S., Bhatia, R., & Kumar, B. (2022). A validated method developed for estimation of Lifitegrast in bulk and pharmaceutical dosage form by UV-Spectrophotometer and RP-HPLC. Austin J. Anal. Pharm. Chem,, 9(1), 1140. https://10.26420/austinjanalpharmchem.2022.1140
  • Scaglione, F., Donde, S., Hassan, T.A., & Jannini, E.A. (2017). Phosphodiesterase type 5 inhibitors for the treatment of erectile dysfunction: pharmacology and clinical impact of the sildenafil citrate orodispersible tablet formulation. Clinical Therapeutics, 39(2), 370-377. https://doi.org/10.1016/j.clinthera.2017.01.001
  • Sutar, A., Magdum, C., Patil, S., & Naikawadi, N. (2008). RP-HPLC estimation of tadalafil in tablet dosage form. Int J Chem Sci, 6(2), 1223-1227. Microsoft Word - PN10-Paper08-1183.doc
  • Xu, Y., Zhong, P., Jiang, A., Shen, X., Li, X., Xu, Z., ... Lei, H. (2020). Raman spectroscopy coupled with chemometrics for food authentication: A review. TRAC Trends in Analytical Chemistry, 131, 116017. https://doi.org/10.1016/j.trac.2020.116017
  • Zakaria, N.I., & Yacob, A.R. (2017). Analysis of Fake Honey and Sildenafil Adulterated Honey. eProceedings Chemistry, 2(1). https://api.semanticscholar.org/CorpusID:79684311

Application of HPLC for detection of sildenafil/tadalafil in marketed honey in Oman

Year 2025, Volume: 12 Issue: 2, 297 - 305

Abstract

Honey adulteration allegedly with phosphodiesterase-5 (PDE-5) inhibitors including sildenafil, and tadalafil is a common and dangerous practice. This study aimed to develop a procedure to detect the presence of common adulterants namely sildenafil and tadalafil using RP-HPLC. Seven commercial honey samples of local and international origin were collected from supermarkets and honey sellers. Both the adulterants in honey samples were identified and quantified with the help of an HPLC technique. Chromatographic separation was done in RP-HPLC mode using buffer: methanol: acetonitrile (5.8: 2.5: 1.7) mobile phase and diode array as a detector. The buffer used was 0.05 M Triethylamine orthophosphate pH (3.0). The results showed that four honey samples (HAD1, HAD5, HAD6, and HAD7) were adulterated with sildenafil, and among them, HAD5 contained the maximum amount of sildenafil as 22.65 mg/g of the honey sample. However, only 2 honey samples HAD4 and HAD6 were found to be adulterated with tadalafil (1.248 and 0.7 mg/g) of the tested honey sample. The result of this study warrants rigorous quality control of the commercially available honey products in Oman by the authorities. The consumption of adulterated honey samples may impact the health of consumers hence further detailed studies must be carried out to confirm the findings of the current study and novel analytical methods be developed to detect the level of other possible adulterants in this valuable product.

Ethical Statement

EBS/PRES0401-COP/04/2022-23 College of Pharmacy, National University of Science and Technology, Azaiba, Muscat, Sultanate of Oman.

Supporting Institution

MoH Sultanate of Oman

Project Number

EBS/PRES0401-COP/04/2022-23

References

  • Abdelshakour, M.A., Salam, R.A.A., Hadad, G.M., Abo-ElMatty, D.M., & Hameed, E.A. A. (2021). HPLC-UV and UPLC-MS/MS methods for the simultaneous analysis of sildenafil, vardenafil, and tadalafil and their counterfeits dapoxetine, paroxetine, citalopram, tramadol, and yohimbine in aphrodisiac products. RSC advances, 11(14), 8055-8064. https://doi.org/10.1039/d0ra10324a
  • Agency, E.M. (1995). ICH Topic Q 2 (R1) validation of analytical procedures: text and methodology. Prescrire International, 20, 278.
  • Al Lawati, H.A., Al Busaidi, I., Kadavilpparampu, A.M., & Suliman, F.O. (2017). Determination of common adulterants in herbal medicine and food samples using core-shell column coupled to tandem mass spectrometry. Journal of Chromatographic Science, 55(3), 232-242. https://10.1093/chromsci/bmw175
  • Ala'Y, S., AlRashdan, Y., Abbasi, N.U., Mostafa, A., Abudayeh, Z., Talhouni, A., & Al-Ebini, Y. (2023). Optimization and validation of HPLC-UV method for the determination of vardenafil, sildenafil, and tadalafil in honey-mixed herbal sachets using a design of experiment. Jordan Journal of Pharmaceutical Sciences, 16(1), 148 162. https://10.35516/jjps.v16i1.1075
  • Bogusz, M.J., Hassan, H., Al-Enazi, E., Ibrahim, Z., & Al-Tufail, M. (2006). Application of LC–ESI–MS–MS for detection of synthetic adulterants in herbal remedies. Journal of Pharmaceutical and Biomedical Analysis, 41(2), 554 564. https://doi.org/10.1016/j.jpba.2005.12.015
  • Cárdenas-Escudero, J., Galán-Madruga, D., & Cáceres, J. (2023). FTIR-ATR detection method for emerging C3-plants-derivated adulterants in honey: Beet, dates, and carob syrups. Talanta, 124768. https://doi.org/10.1016/j.talanta.2023.124768
  • Dou, X., Zhang, L., Chen, Z., Wang, X., Ma, F., Yu, L., ... Li, P. (2023). Establishment and evaluation of multiple adulteration detection of camellia oil by mixture design. Food Chemistry, 406, 135050. https://doi.org/10.1016/j.foodchem.2022.135050
  • Fakhlaei, R., Selamat, J., Khatib, A., Razis, A. F. A., Sukor, R., Ahmad, S., & Babadi, A. A. (2020). The toxic impact of honey adulteration: A review. Foods, 9(11), 1538. https://10.3390/foods9111538
  • FDA. (2022). FDA Warns Four Companies for Selling Tainted Honey-based Products with Hidden Active Drug Ingredients. FDA News Release. https://www.prnewswire.com/news-releases/fda-warns-four-companies-for-selling-tainted-honey-based-products-with-hidden-active-drug-ingredients-301584930.html
  • Gong, B., Ma, M., Xie, W., Yang, X., Huang, Y., Sun, T., ... Huang, J. (2017). Direct comparison of tadalafil with sildenafil for the treatment of erectile dysfunction: a systematic review and meta-analysis. International Urology and Nephrology, 49, 1731-1740. https://doi.org/10.1007/s11255-017-1644-5
  • González-Ceballos, L., Guirado-Moreno, J.C., Utzeri, G., García, J.M., Fernández-Muino, M.A., Osés, S.M., ... Vallejos, S. (2023). Straightforward purification method for the determination of the activity of glucose oxidase and catalase in honey by extracting polyphenols with a film-shaped polymer. Food Chemistry, 405, 134789. https://doi.org/10.1016/j.foodchem.2022.134789
  • Mehryar, L., & Esmaiili, M. (2011). Honey & honey adulteration detection: A review. Proceedings of 11th International Congress on Engineering and Food, NFP1066-libre.pdf
  • Ng, C.M., & Reuter, W.M. (2015). Analysis of Sugars in Honey Using the PerkinElmer Altus HPLC System with RI Detection. Perkin Elmer, Inc, 1 5. https://www.slideshare.net/perkinelmerinc/analysis-of-sugars-in-honey-using-the-perkinelmer-altus-hplc-system-with-ri-detection
  • Pannu, S., Bhatia, R., & Kumar, B. (2022). A validated method developed for estimation of Lifitegrast in bulk and pharmaceutical dosage form by UV-Spectrophotometer and RP-HPLC. Austin J. Anal. Pharm. Chem,, 9(1), 1140. https://10.26420/austinjanalpharmchem.2022.1140
  • Scaglione, F., Donde, S., Hassan, T.A., & Jannini, E.A. (2017). Phosphodiesterase type 5 inhibitors for the treatment of erectile dysfunction: pharmacology and clinical impact of the sildenafil citrate orodispersible tablet formulation. Clinical Therapeutics, 39(2), 370-377. https://doi.org/10.1016/j.clinthera.2017.01.001
  • Sutar, A., Magdum, C., Patil, S., & Naikawadi, N. (2008). RP-HPLC estimation of tadalafil in tablet dosage form. Int J Chem Sci, 6(2), 1223-1227. Microsoft Word - PN10-Paper08-1183.doc
  • Xu, Y., Zhong, P., Jiang, A., Shen, X., Li, X., Xu, Z., ... Lei, H. (2020). Raman spectroscopy coupled with chemometrics for food authentication: A review. TRAC Trends in Analytical Chemistry, 131, 116017. https://doi.org/10.1016/j.trac.2020.116017
  • Zakaria, N.I., & Yacob, A.R. (2017). Analysis of Fake Honey and Sildenafil Adulterated Honey. eProceedings Chemistry, 2(1). https://api.semanticscholar.org/CorpusID:79684311
There are 18 citations in total.

Details

Primary Language English
Subjects Pharmaceutical Chemistry
Journal Section Articles
Authors

Hameda Hamood Al Dhakhri This is me 0009-0002-7687-2908

Fatema Alqassabi This is me 0009-0003-4275-1574

Israa Alrasbi This is me 0009-0009-2492-5554

Dhuha Alhinai This is me 0009-0002-2421-8090

Salha Al Salty This is me 0009-0008-8206-4468

Sumit Pannu This is me 0009-0003-8177-0815

Shaima Al Balushi This is me 0009-0004-1420-7376

Shah Alam Khan This is me 0000-0002-0729-3403

Mohammad Jawaıd Akhtar 0000-0002-9460-5304

Project Number EBS/PRES0401-COP/04/2022-23
Early Pub Date March 19, 2025
Publication Date
Submission Date July 18, 2024
Acceptance Date December 11, 2024
Published in Issue Year 2025 Volume: 12 Issue: 2

Cite

APA Al Dhakhri, H. H., Alqassabi, F., Alrasbi, I., Alhinai, D., et al. (2025). Application of HPLC for detection of sildenafil/tadalafil in marketed honey in Oman. International Journal of Secondary Metabolite, 12(2), 297-305.
International Journal of Secondary Metabolite

e-ISSN: 2148-6905