Identification and Quantification of an Adulterant in a Dietary Supplement Marketed for Sexual Enhancement

Redko, Flavia; Flor, Sabrina; Lucangioli, Silvia; Ulloa, Jerónimo Luis; Ricco, Rafael A.; Fernández, Claudio Alejandro; Sambrotta, Luis; Muschietti, Liliana

doi:10.14302/issn.2328-0182.japst-18-2344

Cited by 4 publications

(10 citation statements)

References 24 publications

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“…This study represents the first report in Latin America and one of the few independent studies of an adulteration with an unapproved PDE‐5i of a DS for the treatment of ED 26 . Recently, we have also reported the identification and quantification, using HPLC‐tandem mass spectrometry (MS/MS), of tadalafil as an adulterant in a DS marketed in Argentina for sexual enhancement 27 . Mustazza et al 28 detected the presence of sildenafil analogues in an illegal supplement, but more importantly the authors also reported extensive spectral data on mass fragmentation and NMR chemical shifts of sildenafil, thiosildenafil, acetildenafil, and 13 of their analogues, and provide comprehensive information on the route of synthesis for the benefit of those laboratories that need to synthesize analogue reference standards in‐house.…”

Section: Resultsmentioning

confidence: 80%

Adulterants in selected dietary supplements and their detection methods

Muschietti

Redko

Ulloa

2020

Drug Testing and Analysis

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At present, there is a growing trend toward the intentional adulteration of dietary supplements (DS) with synthetic pharmaceuticals, which represents an alarming emerging risk to consumers and a serious problem for regulatory agencies. An amazing array of synthetic drugs and their analogues have been reported as adulterants in DS. Mainly, the presence of analogues represents a serious health risk as their efficacy and toxic effects have not been clinically assessed yet and may result in unpredictable adverse effects. The purpose of this review is to provide an overview, over the period 2009–2019, of the most frequently reported adulterants in DS for the treatment of erectile dysfunction, obesity/overweight, diabetes mellitus, and hypertension and the analytical methods used for their detection.

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Section: Resultsmentioning

confidence: 80%

Adulterants in selected dietary supplements and their detection methods

Muschietti

Redko

Ulloa

2020

Drug Testing and Analysis

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“…In Romania, the National Agency for Medicine and Medical Devices of Romania (NAMMDR) lists sildenafil medicinal products of the following therapeutic strengths: 25, 50, and 100 mg. The adverse effects related to sildenafil consumption include headache, flushing, dizziness, dyspepsia, nasal congestion, and altered vision [ 4 , 5 , 6 ]. Furthermore, disturbed color vision and temporary effects on the electroretinogram (ERG) were reported [ 7 ].…”

Section: Introductionmentioning

confidence: 99%

“…This practice of adulterating food supplements for both potency and losing weight is a common phenomenon worldwide [ 4 ]. Moreover, the risk of harm is increased by adding synthetic drugs and various impurities [ 6 ].…”

Section: Introductionmentioning

confidence: 99%

“…Given that the adulteration of dietary supplements is a major problem by putting consumers at risk, a short review of the literature was undertaken in order to identify the analytical methods of extraction of the interest compounds from various herbal products, as well as their determination. The literature survey revealed a wide range of analytical techniques employed for the detection and determination of interest compounds in herbal products, including GC-MS (gas chromatography–mass spectrometry), LC-MS (liquid chromatography–mass spectrometry), HPLC (high-performance liquid chromatography), NMR (nuclear magnetic resonance) spectroscopy, vibrational spectroscopy, LC-FT-ICR-MS (liquid chromatography–Fourier transform ion cyclotron resonance–mass spectrometry), liquid chromatograph–hybrid triple quadrupole linear ion trap mass spectrometer with an information-dependent acquisition, UHPLC-TOF-MS (ultra-high performance liquid chromatography–time of flight–mass spectrometry), IMS (ion mobility spectroscopy), and immunoassay methods [ 2 , 5 , 6 , 8 , 30 , 31 ]. A brief description of the analyzed methods along with the targeted analyte is described below.…”

Section: Introductionmentioning

confidence: 99%

“…The study described the detection of spots with UV light (254 and 366 nm) and via derivatization with Draggendorff and anisaldehyde/sulfuric acid reagents. This was followed by the identification of tadalafil via various spectroscopic techniques, such as mono- and bi-dimensional nuclear magnetic resonance (using dimethylsulfoxide-D6 as the solvent), Fourier-transform infrared (FT-IR) spectroscopy, and mass spectrometry [ 6 ]. Quantification of tadalafil was performed via high-performance liquid chromatography–mass spectrometry (HPLC-MS/MS) [ 6 ].…”

Section: Introductionmentioning

confidence: 99%

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Determination of Phosphodiesterase Type-5 Inhibitors (PDE-5) in Dietary Supplements

et al. 2023

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This study proposed a high-performance thin-layer chromatography (HPTLC) screening method to detect phosphodiesterase 5 (PDE-5) inhibitors as possible adulterant agents in various dietary supplements. Chromatographic analysis was performed on silica gel 60F254 plates using a mixture of ethyl acetate:toluene:methanol:ammonia in a volume ratio of 50:30:20:0.5 as a mobile phase. The system provided compact spots and symmetrical peaks of sildenafil and tadalafil with retardation factor values of 0.55 and 0.90, respectively. The analysis of products purchased from the internet or specialized stores demonstrated the presence of sildenafil, tadalafil, or both compounds in 73.3% of products, highlighting inadequacies and inconsistencies in the labeling, as all dietary supplements were declared to be natural. The results were confirmed using ultra-high-performance liquid chromatography coupled with a positive electrospray ionization high-resolution tandem mass spectrometry (UHPLC-HRMS-MS) method. Furthermore, in some samples, vardenafil and various analogs of PDE-5 inhibitors were detected using a non-target HRMS-MS approach. The results of the quantitative analysis revealed similar findings between the two methods, with adulterant quantities found to be similar to or higher than those in approved medicinal products. This study demonstrated that the HPTLC method is a suitable and economical method for screening PDE-5 inhibitors as adulterants in dietary supplements intended for sexual activity enhancement.

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Screening results for non-declared synthetic phosphodiesterase-5 inhibitors being added to dietary supplements of plant origin

Перова¹,

Эллер²,

Tumol`skaya³

2019

Health Risk Analysis

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Non-declared addition of synthetic phosphodiesterase-5 inhibitors (PDE-5 inhibitors) to dietary supplements (DS) of plant origin in order to stimulate potency is a serios problem. Such counterfeiting strengthens therapeutic effects produced by a product; similar effects can't occur only due to components of DS of plant origin. Synthetic PDE-5 inhibitors are both substances of official medications and their structural analogues. When synthetic PDE-5 inhibitors are consumed as components in DS in order to increase potency, it can be hazardous for consumers' health due to unpredictable or even lethal side effects. Our research goal was to reveal concentrations of non-declared synthetic PDE-5 inhibitors in DS consumed by males. Our research objects were 175 DS selected by Rospotrebnadzor in different Russian regions. Synthetic PDE-5 inhibitors were detected in samples by HPLC with diode array spectrophotometric detection and MS-detection as per guidelines developed by us and approved on by Rospotrebnadzor (MG 4.1.3331-16). Our research revealed that 36% of DS that were consumed to increase potency contained non-declared synthetic PDE-5 inhibitors with Tadalafil and Sildenafil being the most widely spread ones 42.9% and 28.6% of all counterfeit cases). Their combination or analogues of PDE-5 inhibitors were detected significantly less frequently; complicated mixtures containing three or more components were also rather rare. Contents of Tadalafil, Sildenafil, or Vardenafil in DS varied from trace quantities to concentrations that corresponded to recommended daily doses for these medications or even higher than such doses. We identified derivatives of Sildenafil and Tadalafil among PDE-5 inhibitors; their quantities varied from 1.2 mg/capsule to 24.3 mg/capsule. The developed procedure allowed detecting counterfeited DS with not only Tadalafil, Sildenafil, or Vardenafil being added to them, but also analogues of synthetic PDE-5 inhibitors.

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Identification and Quantification of an Adulterant in a Dietary Supplement Marketed for Sexual Enhancement

Cited by 4 publications

References 24 publications

Adulterants in selected dietary supplements and their detection methods

Adulterants in selected dietary supplements and their detection methods

Determination of Phosphodiesterase Type-5 Inhibitors (PDE-5) in Dietary Supplements

Screening results for non-declared synthetic phosphodiesterase-5 inhibitors being added to dietary supplements of plant origin

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