Lifestyle illicit drug seizures: A routine ESI–LC–MS method for the identification of sildenafil and vardenafil

Patterson, R. E.; Mabe, Phillip J.; Mitchell, E. Nicole; Cory, Wendy

doi:10.1016/j.forsciint.2012.05.003

Cited by 12 publications

(3 citation statements)

References 26 publications

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“…In the last decade, LC coupled to MS detection has become a primary tool in the analysis of adulterants in PFS, since it combines the separation capacity of LC with the sensitivity and selectivity of MS detectors allowing for molecular identification (Patterson and others ; Vaclavik and others , ). When standards are available, the use of LC preceding MS analysis also contributes to the identification of compounds based on its retention time.…”

Section: Determination Of Adulterating Substancesmentioning

confidence: 99%

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Rocha

Amaral

Oliveira

2015

Comp Rev Food Sci Food Safe

193

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In the last few years, the consumption of dietary supplements, especially those having plants as ingredients, has been increasing due to the common idea that they are natural products posing no risks to human health. In the European Union and the United States, dietary supplements are legally considered as foods/special category of foods, thus are not being submitted to any safety assessment prior to their commercialization. Among the issues that can affect safety, adulteration by the illegal addition of pharmaceutical substances or their analogs is of major concern since unscrupulous producers can falsify these products to provide for quick effects and to increase sales. This review discusses the various classes of synthetic drugs most frequently described as being illegally added to dietary supplements marketed for weight loss, muscle building/sport performance and sexual performance enhancement. Information regarding regulation and consumption is also presented. Finally, several conventional and advanced analytical techniques used to detect and identify different adulterants in dietary supplements and therefore also in foods, with particular emphasis on plant food supplements, are critically described. This review demonstrates that dietary supplement adulteration is an emerging food safety problem and that an effective control by food regulatory authorities is needed to safeguard consumers.

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Section: Determination Of Adulterating Substancesmentioning

confidence: 99%

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Rocha

Amaral

Oliveira

2015

Comp Rev Food Sci Food Safe

193

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“…Consumer demand for dietary supplements that support healthy lifestyles has steadily increased worldwide. In the last decade, illegal adulterants of pharmaceuticals, unapproved drugs, and prohibited ingredients have increased and posed a global challenge in safety control of dietary supplements [ 1 ]. The easy access of Internet, overseas direct purchase, along with an increasingly complex global supply chain, has led to the widespread illegal drug distribution worldwide [ 2 ].…”

Section: Introductionmentioning

confidence: 99%

Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

et al. 2020

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In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

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“…[26][27][28][29][30][31] Liquid chromatographyquadrupole-time of flight mass spectrometry (LC-QTOF-MS) carried out in full scan mode can be used to elucidate the accurate mass of target and nontarget compounds, as well as that of unknown compounds, while the multiple reaction monitoring (MRM) mode can be used only to detect the mass of target compounds. Fragmentation patterns can be used to determine the structure of unknown components by interpreting the product ions.…”

Section: Introductionmentioning

confidence: 99%

Identification and evaluation of fragmentation pathways of PDE-5 inhibitor analogues using LC-QTOF-MS

Do¹,

Noh²,

Yoon³

et al. 2015

Analytical Science and Technology

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Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction.In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatographyquadrupole-time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions.Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.

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Lifestyle illicit drug seizures: A routine ESI–LC–MS method for the identification of sildenafil and vardenafil

Cited by 12 publications

References 26 publications

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Identification and evaluation of fragmentation pathways of PDE-5 inhibitor analogues using LC-QTOF-MS

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