Screening of Phosphodiesterase-5 Inhibitors and Their Analogs in Dietary Supplements by Liquid Chromatography–Hybrid Ion Trap–Time of Flight Mass Spectrometry

Kim, Unyong; Cho, Hyun-Deok; Kang, Minah; Suh, Joon Hyuk; Eom, Han Young; Kim, Jung-Hyun; Seo, Sumin; Kim, Gunwoo; Koo, Hye Ryoung; NaRy, Ha; Song, Un Tak; Han, Sang Beom

doi:10.3390/molecules25122734

Cited by 8 publications

(4 citation statements)

References 41 publications

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“…In addition, developing efficient methods to detect PDE5-is and any analogue whatever structure, that is based on activity, may be useful. The USA, Canada, the Czech Republic, Korea and China have developed rapid analytical tests in line with this idea [58,59,[73][74][75][76]. Thus, several supplements can be simultaneously tested and rapidly removed from the market if proven adulterated.…”

Section: Prevention Measuresmentioning

confidence: 99%

Drug adulteration of sexual enhancement supplements: a worldwide insidious public health threat

Yéléhé‐Okouma

Pape

Humbertjean

et al. 2021

Fundamemntal Clinical Pharma

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Worldwide, the consumption of dietary supplements for the enhancement of sexual performance is common. Consumers are generally fond of these products because they often want to avoid drugs, preferring “natural” than “chemical” solutions. This is challenging, as many of these supplements labelled “herbal” or “natural” are actually adulterated with drugs, mainly phosphodiesterase‐5 inhibitors. This phenomenon is facilitated by fewer demanding regulations for marketing supplements. Thus, consumers may be widely exposed to serious adverse events, such as acute liver injury, kidney failure, pulmonary embolism, stroke or even death. We aim to warn physicians about this issue. This multidisciplinary review simultaneously deals with clinical consequences of this phenomenon, analytical toxicology and regulation. Indeed, after outlining this worldwide issue and highlighting that a drug‐adulterated dietary supplement is actually a falsified drug, we discuss its main contributing factors. Then, we describe some examples of adverse events of which a case of sildenafil–tadalafil‐induced ischaemic stroke that benefited medical care in our hospital. Furthermore, we present some means to avoid adulteration and discuss their limitations that may be explained by the heterogeneity of the regulation of dietary supplements between countries. Doing so, we point out the requirement of a global harmonization of this regulation for an efficient eradication of this public health threat. Meanwhile, dietary supplements should be considered adulterated until proven otherwise. Thus, we encourage physicians to investigate these products in the drug histories of their patients, especially when clinical conditions cannot be explained by classical aetiologies.

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Section: Prevention Measuresmentioning

confidence: 99%

Drug adulteration of sexual enhancement supplements: a worldwide insidious public health threat

Yéléhé‐Okouma

Pape

Humbertjean

et al. 2021

Fundamemntal Clinical Pharma

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“…HPLC–UV has been successfully applied in screening analysis when each drug shows a unique UV absorption profile while having limits on the identification of new derivatives (Dahshan et al, 2019). Mass spectrometry‐based methods could provide more details for structural information but still need reference standards as controls (Kim et al, 2020; Lee et al, 2020; Li et al, 2020). It is difficult to curb tailor‐made designer drugs from clandestine laboratories owing to patent disclosure issues and a lack of available scientific publications.…”

Section: Introductionmentioning

confidence: 99%

A novel standard‐free detection of adulteration method for sildenafil derivatives in dietary supplements

Lv,

Wang,

et al. 2024

Biomedical Chromatography

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The rapid and accurate detection of illegal adulteration of chemical drugs into dietary supplements is a big challenge in the food chemistry field. Detection of compounds without a standard reference is even more difficult; however, this is a common situation. Here in this study, a novel “standard‐free detection of adulteration” (SFDA) method was proposed and phosphodiesterase‐5 inhibitor derivatives were used as an example to figure out the possibility and reliability of this SFDA method. After analysis by quadrupole coupled time of flight–tandem mass spectrometry detection and multivariable statistics, six common fragment ions were chosen to indicate whether adulteration was present or not, while 20 characteristic fragment ions indicated whether adulteration was by nitrogen‐containing heterocycles or by anilines. Furthermore, the quantitative methods were conducted by high‐performance liquid chromatography–tandem mass spectrometry. In a word, this strategy allows for a quick determination of dietary supplement adulteration without any need for standard materials, improving the efficacy of food safety testing.

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“…The LC-MS technique is sensitive and selective for target substances in complex matrices without extensive sample preparation procedures [28]. LC-MS also has the advantage of combining online optical detectors to obtain the ultraviolet spectrum and mass spectrum simultaneously.…”

Section: Introductionmentioning

confidence: 99%

Development of a Robust Method for Screening PDE-5 Inhibitor Additives in Dietary Supplements Using UPLC-MS/MS

Wang

2023

AJACR

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A novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method was developed to detect the illegal additive of phosphodiesterase type 5 (PDE-5) inhibitors in dietary supplements. With the optimized chromatographic program, vardenafil, sildenafil, and tadalafil were separated within 5 minutes. The MS1, MS2, and retention time of PDE-5 inhibitors were acquired simultaneously within the information dependent acquisition mass spectrometry mode. Quantification was achieved via the quantity ion current chromatogram that was extracted from the total ion current. The linear range of vardenafil and sildenafil was 0.5-48 mg/L while the range of tadalafil was 0.3-36 mg/L. The correlation coefficients of the calibration curves of three PDE-5 inhibitors were all greater than 99.9%. At three concentration levels, the RSD values of the five repeat tests were all better than 1.30%. Sildenafil was detected in one dietary supplement. The comprehensive method of this study is reliable and may be a powerful tool for routine PDE-5 inhibitor screening and determination.

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Screening of Phosphodiesterase-5 Inhibitors and Their Analogs in Dietary Supplements by Liquid Chromatography–Hybrid Ion Trap–Time of Flight Mass Spectrometry

Cited by 8 publications

References 41 publications

Drug adulteration of sexual enhancement supplements: a worldwide insidious public health threat

Drug adulteration of sexual enhancement supplements: a worldwide insidious public health threat

A novel standard‐free detection of adulteration method for sildenafil derivatives in dietary supplements

Development of a Robust Method for Screening PDE-5 Inhibitor Additives in Dietary Supplements Using UPLC-MS/MS

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