Simultaneous determination of 38 phosphodiestrase-5 inhibitors in illicit erectile dysfunction products by liquid chromatography–electrospray ionization-tandem mass spectrometry

Lee, Eung-Sun; Lee, Ji Hyun; Han, Kyoung Moon; Kim, Ji Won; Hwang, In-Sul; Cho, Soo-Yeul; Han, Soon Young; Kim, Jin-Ho

doi:10.1016/j.jpba.2013.05.009

Cited by 44 publications

(18 citation statements)

References 22 publications

(46 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Adulteration is an exemplary repercussion of such laxity. Well documented are instances of diuretics, stimulants, anorectics, or oxidative uncouplers contained in weight loss supplements [60][61][62][63][64][65][66][67][68][69][70][71][72][73][74], steroids in performance enhancers [75][76][77][78][79][80], and phosphodiesterase 5 inhibitors contained within male enhancement products [72,74,[81][82][83][84][85][86][87][88][89][90][91][92][93]. At least nine people died in Sweden following exposure to Kratom adulterated with Odesmethyltramadol, a potent opioid analgesic.…”

Section: Supplement Regulationmentioning

confidence: 99%

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

et al. 2016

View full text Add to dashboard Cite

Introduction Kratom (Mitragyna speciosa), a plant native to Southeast Asia, has been used for centuries for its stimulant and opium-like effects. Mitragynine and 7-hydroxymitragynine, exclusive to M. speciosa, are the alkaloids primary responsible for Kratom's biologic and psychoactive profile, and likely contribute to its problematic use. We purchased several commercially available Kratom analogs for analysis and through our results, present evidence of probable adulteration with the highly potent and addictive plant alkaloid, 7-hydroxymitragynine. Methods A simple and sensitive LC-MS/MS method was developed for simultaneous quantification of mitragynine and 7-hydroxymitragynine in methanol extract of marketed Kratom supplements. Results We found multiple commercial Kratom products to have concentrations of 7-hydroxymitragynine that are substantially higher than those found in raw M. speciosa leaves. Conclusions We have found multiple packaged commercial Kratom products likely to contain artificially elevated concentrations of 7-hydroxymitragynine, the alkaloid responsible for M. speciosa's concerning mechanistic and side effect profile. This study describes a unique form of product adulteration, which stresses the importance of increased dietary supplement oversight of Kratom-containing supplements.

show abstract

Section: Supplement Regulationmentioning

confidence: 99%

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

et al. 2016

View full text Add to dashboard Cite

show abstract

“…Such approach does not provide as high level of identification reliability as is achieved by comparisons with standards, but it was considered acceptable for the purpose of screening and more economical than purchasing many standards. The LC/MS data was searched for the accurate masses (±25 ppm window) of 67 PDE5 inhibitors listed in recent review articles focused on this class of drugs [15,16] (extracted ion chromatograms and corresponding structures are given in Supporting Information). Positive samples are summarized in Table 1.…”

mentioning

confidence: 99%

“…For most of the detected PDE5 inhibitors, the CID fragments matched those reported in the literature. [15,16] In a few cases, it took more effort to conclude about the identity of the observed species. In the CID spectra of ions with m/z corresponding to protonated cinnamyldenafil (samples #2 and #3, mass errors 3.1 and 2.9 ppm, respectively, Table 1), only one product ion (m/z 117) was observed of the two reported in the literature (m/z 115 and 117).…”

mentioning

confidence: 99%

“…In the CID spectra of ions with m/z corresponding to protonated cinnamyldenafil (samples #2 and #3, mass errors 3.1 and 2.9 ppm, respectively, Table 1), only one product ion (m/z 117) was observed of the two reported in the literature (m/z 115 and 117). [16] The spectra, identical in both samples #2 and #3 ( Fig. 1(a)), were therefore manually interpreted ( Fig.…”

mentioning

confidence: 99%

“…Ref [15] . b Ref [16] ; only two most abundant ions are indicated in the study. c Spectrum interpreted manually, refer to the text.…”

mentioning

confidence: 99%

See 2 more Smart Citations

Screening of synthetic phosphodiesterase‐5 inhibitors in herbal dietary supplements using transmission‐mode desorption electrospray and high‐resolution mass spectrometry

et al. 2016

View full text Add to dashboard Cite

Fast ultra‐high‐performance liquid chromatography with diode array and mass spectrometry method for determination of tadalafil drug substance and its impurities

Schreiber

Halko

Hutta

2017

Biomedical Chromatography

View full text Add to dashboard Cite

Tadalafil is used for the treatment of erectile dysfunction. Its related patents expired in 2016, and so related generic drug production is predicted to be increased. This work is focused on developing a fast ultra-high-performance liquid chromatography with diode array detection and/or mass spectrometry detection for the separation and determination of tadalafil and its impurities in pharmaceutical samples. A modern reversed-phase stationary phase with sub-2 μm particle size, Zorbax StableBond Rapid Resolution High Definition with octylsilane chemically bonded phase to totally porous silica particles, was used for the solving this problem. Column temperature was set at 40 ± 0.1°C. A mobile phase consisting of acetonitrile and aqueous solution of 0.1% (v/v) trifluoroacetic acid for diode array detection detection and 0.05% (v/v) formic acid, both running at a flow rate of 0.62 mL/min, were used to achieve the required separation of all components within a 5 min run. The limit of detection was 3.5 μg/L and the limit of quantification was 10.0 μg/L for the method for both UV and MS detectors. Accurate mass spectra of tadalafil's related impurities are shown for advanced confirmation. The method is directly transferable to routine analysis of tadalafil in pharmaceutical and control laboratories.

show abstract

Simultaneous determination of 38 phosphodiestrase-5 inhibitors in illicit erectile dysfunction products by liquid chromatography–electrospray ionization-tandem mass spectrometry

Cited by 44 publications

References 22 publications

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

Screening of synthetic phosphodiesterase‐5 inhibitors in herbal dietary supplements using transmission‐mode desorption electrospray and high‐resolution mass spectrometry

Fast ultra‐high‐performance liquid chromatography with diode array and mass spectrometry method for determination of tadalafil drug substance and its impurities

Contact Info

Product

Resources

About