, Volume 81, Issue 5, pp 777–783 | Cite as

HPLC–UV Chromatographic Methods for Detection and Quantification of Undeclared Withdrawn Synthetic Medications in Counterfeit Herbal Medicines with Confirmation by HPLC–PDA and Mass Spectrometry

  • A. Hemdan
  • Shereen M. Tawakol


Adulteration of herbal medicinal products with synthetic pharmaceuticals remains a serious problem. The purpose of this study is to develop a procedure for determination of some common synthetic adulterants in some herbal remedies available on the market, utilizing a reversed-phase high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection. Herbal medicines for weight loss and another for erectile dysfunction were tested for presence of conceivable adulterants. The weight loss products were discovered to be defiled with the effectively withdrawn drug sibutramine (SIB) and with phenolphthalein (PPH), which has been demonstrated to cause tumors. On the other hand, sildenafil (SLD), a medication contraindicated for patients with heart diseases (sometimes causing serious side-effects with respect to blood pressure), was found in the herbal product for erectile dysfunction. The mobile phase for quantification of sibutramine and phenolphthalein was acetonitrile–potassium hydrogen phosphate buffer (pH 3) adjusted using o-phosphoric acid (40/60 v/v) with detection at 223 nm. Meanwhile, the mobile phase for sildenafil was acetonitrile–potassium hydrogen phosphate buffer (pH 3.2) adjusted using o-phosphoric acid (50/50 v/v) with detection at 230 nm. Presence of the adulterants was confirmed using LC–photodiode array (PDA) and mass spectrometry.

Graphical Abstract


LC–PDA MS/MS Herbal medicines Adulteration Sibutramine Sildenafil 



The authors received no funding to carry out this study.

Compliance with Ethical Standards

Conflict of interest

The authors declare that they have no conflicts of interest.

Human animal rights

This article does not contain any studies with human participants or animals performed by any of the authors.

Supplementary material

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Department of Pharmaceutical Analytical Chemistry, Faculty of PharmacyAhram Canadian University6th of OctoberEgypt
  2. 2.Department of Pharmaceutical Analytical Chemistry, Faculty of PharmacyHelwan UniversityHelwanEgypt

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