Detection of 94 compounds related to sexual enhancement including sildenafil, tadalafil, vardenafil and their analogues in various formulations of dietary supplements and food samples using HPLC and LC-MS/MS

Min, A Young; Park, Ok Rim; Han, Ji Hye; Yang, Yoon Ji; Kim, Hyung-Il; Lee, Ji Hyun

doi:10.1080/19440049.2021.1881623

Cited by 8 publications

(3 citation statements)

References 26 publications

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“…There have been several analytical studies on these compounds over the years, and these studies have generally used highperformance liquid chromatography (HPLC) and mass spectrometry (MS). [10][11][12] However, analytical data that can be used for the accurate screening and identification of potential adulterants without employing reference standards are lacking. The categories of illegal substances, which now include erectile dysfunction drugs, weight-loss drugs, and anti-osteoporosis and anti-gout drugs, are increasing, and substances with structures similar to those of the original drugs continue to emerge.…”

Section: Introductionmentioning

confidence: 99%

“…There have been several analytical studies on these compounds over the years, and these studies have generally used high‐performance liquid chromatography (HPLC) and mass spectrometry (MS) 10–12 . However, analytical data that can be used for the accurate screening and identification of potential adulterants without employing reference standards are lacking.…”

Section: Introductionmentioning

confidence: 99%

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Intercomparison study of fragmentation pathways and fragment ion structures for screening of illegal drugs and their novel analogues used to adulterate dietary supplements using liquid chromatography/quadrupole time‐of‐flight mass spectrometry

Kim

Choi

Lim

et al. 2022

Rapid Comm Mass Spectrometry

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Rationale As public interest in health and immunity has increased in recent years, so has the demand for dietary supplements. However, supplements adulterated with illegal drugs and their novel analogues are being sold even as the pharmacological efficacies of these drugs are being advertised. Since the use of these illegal compounds can have serious side effects, they pose a risk to public health. Hence, in this study, we propose a strategy for proactively testing drugs and novel analogues that may be added to dietary supplements illegally. Methods The optimal conditions for liquid chromatography/quadrupole time‐of‐flight mass spectrometry were explored to determine the fragmentation patterns for 60 compounds. The optimal conditions were established by comparing the areas and heights of the precursor ion peaks at a fragmentor voltage of 125 or 175 V. Furthermore, the optimized spectra were acquired using collision energies of 1 to 50 eV. The energy value was selected based on the condition that the mass error of the precursor ions is 10 ppm or lower. Results The fragmentation pathway of each product ion and its chemical structure were predicted and determined. In addition, the obtained structural information was used to screen 18 seized samples. Based on the precursor ions and the corresponding fragmentation patterns, the unknown compounds present in the samples were identified as desulfonylchlorosildenafil and propoxyphenylthiohydroxy homosildenafil. Conclusions We obtained mass spectrometry‐based information for various compounds by predicting the fragmentation pathways and chemical structures of their fragment ions. Subsequently, based on the obtained structural information, we tested several seized samples and were able to detect two novel analogues in four of the samples. Therefore, the proposed approach is suitable for quickly and accurately identifying the unknown compounds detected in real‐world samples.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Intercomparison study of fragmentation pathways and fragment ion structures for screening of illegal drugs and their novel analogues used to adulterate dietary supplements using liquid chromatography/quadrupole time‐of‐flight mass spectrometry

Kim

Choi

Lim

et al. 2022

Rapid Comm Mass Spectrometry

Self Cite

View full text Add to dashboard Cite

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“…In recent years, research in different countries on FS has focused mainly on quality assessment, including the determination of the content of impurities such as mercury [ 4 , 5 ], arsenic [ 6 ], cyanotoxins [ 7 ], polycyclic aromatic hydrocarbons [ 8 ], as well as drug components that should not be present in FS, such as potency substances [ 9 ] and pharmaceutical adulterants, such as anxiolytics, antidepressants, anorexics, stimulants and laxatives [ 10 ]. A significant problem that is not addressed in scientific research is incorrect content of the declared ingredients in FS.…”

Section: Introductionmentioning

confidence: 99%

Quality of Calcium Food Supplements: Evaluation Compared to Manufacturers’ Declarations

et al. 2022

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Calcium (Ca) is a macronutrient necessary for the proper functioning of an organism. In the case of insufficient consumption with diet, its deficiencies can be supplemented with food supplements (FS). These supplements are used, for example, as an auxiliary in the prevention of osteoporosis, allergies, hair loss or nail brittleness. The purpose of the study was to assess the compliance of Ca content with the manufacturers’ declaration. The material consisted of 108 FS. Ca content was determined by atomic absorption spectrometry (AAS). It was shown that 1.9% of the samples were characterized by a Ca content that was too low in comparison to the manufacturer’s declaration, while a content that was relatively too high was found in 54.6% of FS. The quality of FS should be monitored to ensure patient safety.

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Rapid detection of multiple sildenafil and tadalafil adulterants in dietary supplements by dual-labeled probe time-resolved fluorescence immunochromatography assay

Wei,

Zhang,

Huang

et al. 2024

Food Bioscience

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Detection of 94 compounds related to sexual enhancement including sildenafil, tadalafil, vardenafil and their analogues in various formulations of dietary supplements and food samples using HPLC and LC-MS/MS

Cited by 8 publications

References 26 publications

Intercomparison study of fragmentation pathways and fragment ion structures for screening of illegal drugs and their novel analogues used to adulterate dietary supplements using liquid chromatography/quadrupole time‐of‐flight mass spectrometry

Intercomparison study of fragmentation pathways and fragment ion structures for screening of illegal drugs and their novel analogues used to adulterate dietary supplements using liquid chromatography/quadrupole time‐of‐flight mass spectrometry

Quality of Calcium Food Supplements: Evaluation Compared to Manufacturers’ Declarations

Rapid detection of multiple sildenafil and tadalafil adulterants in dietary supplements by dual-labeled probe time-resolved fluorescence immunochromatography assay

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