HPLC–UV Chromatographic Methods for Detection and Quantification of Undeclared Withdrawn Synthetic Medications in Counterfeit Herbal Medicines with Confirmation by HPLC–PDA and Mass Spectrometry
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 The weight loss products were discovered to be defiled with the effectively withdrawn drug sibutramine (SIB) and with phenolphthalein (PPH), which has been demonstrated to cause tumors.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.
KeywordsLC–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.
- 1.Guidelines for the Appropriate Use of Herbal Medicines (1998) WHO Regional Publications, WHO Regional Office for The Western Pacific, ManilaGoogle Scholar
- 2.WHO Guidelines on Safety Monitoring of Herbal Medicines in Pharmacovigilance Systems, WHO, Geneva, 2004Google Scholar
- 3.Kasilo OMJ, Trapsida JM (2011) Afr Health Mon (Special Issue) 14:25–31Google Scholar
- 4.Ernst E, Pittler MH (2002) Complement Altern Med 86:149–161Google Scholar
- 5.Ernst E (2000) In: Dukes MNG, Aronson JK (eds) Meyler’s side effects of drugs, 14th edn. Elsevier Science, Amsterdam, pp 1649–1681Google Scholar
- 6.Johns A (2008) Nature, 451Google Scholar
- 7.Mills S, Bone K (2005) The essential guide to herbal safety. Elsevier, Maryland HeightsGoogle Scholar
- 19.Indications and Clinical Use, Product Monograph of VIAGRA (sildenafil citrate), Revised in 26 August 2013Google Scholar
- 20.Blachut D, Siwinska-Ziolkowska A, Szukalski B, Wojtassiewicz K, Czarnocki Z, Kobylecka A, Bykas-Strekowska M (2007) Prob Forensic Sci 70:225–235Google Scholar
- 22.Wei M, Tao P, Ming-Da Z, Xiao-Juan L, Qiang M, Dong-Dong C, Li L, Wei G, Ying-Zhang T (2009) Chin J Anal Chem 37:1583–1589Google Scholar
- 26.Mu-changseng T, Hueilun J (2002) J Food Drug Anal 10(2):112–119Google Scholar
- 28.Liang Q, Qu J, Luo G, Wang Y (2005) J Pharm Biomed Anal 2005, online at www.sciencedirect.com
- 31.Kanan S, Abu-Yousef IA, Gunasekar C, Abdo N, Narasimhan S (2009) Eur J Sci Res 34:348–357Google Scholar
- 32.Kamil M, Naji MA (2011) VIVECHAN-IJR. 2Google Scholar
- 35.[Dietary supplements: What you need to know. Office of Dietary Supplements. http://ods.od.nih.gov/pubs/DS_WhatYouNeedToKnow.pdf. Accessed 15 Sept 2014. Tips for dietary supplement users. U.S Food and Drug Administration]
- 36.[http://www.fda.gov/Food/DietarySupplements/UsingDietarySupplements/ucm110567.htm. Accessed 15 Sept 2014.]
- 37.ICH (2005) Validation of analytical procedures: text and methodology Q2 (R1). International Conference on Harmonization; 2005; GenevaGoogle Scholar