Rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography–triple quadrupole mass spectrometry

Mokhtar, Siti Umairah; Chin, Sung‐Tong; Kee, Chee‐Leong; Low, Min‐Yong; Drummer, Olaf H.; Marriott, Philip J.

doi:10.1016/j.jpba.2016.01.034

Cited by 43 publications

(20 citation statements)

References 31 publications

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“…The retention times and mass errors of all analytes are listed in Table 1, and the extracted ion chromatograms are depicted in Figure 1. (6), piperidinohongdenafil (7), homosildenafil (8), dimethylsildenafil (9), udenafil (10), cyclopentinafil (11), thiosildenafil (12), hydroxythiohomosildenafil (13), thiohomosildenafil (14), dimethylthiosildenafil (15), oxohongdenafil (16), benzylsildenafil (17), hydroxychlorodenafil (18), chlorodenafil (19), nitrodenafil (20), nor-neosildenafil (21), dichlorodenafil (22), vardenafil (23), acetylvardenafil (24), hydroxyvardenafil (25), nor-neovardenafil (26), desulfovardenafil (27), pseudovardenafil (28), tadalafil (29), aminotadalafil (30), acetaminotadalafil (31), demethyltadalafil (32), chloropretadalafil (33), N-octyltadalafil (34), yohimbine (35), mirodenafil (36), thioquinapiperifil (37), xanthoanthrafil (38), and phenolphthalein (39). * indicated the analytes among multiple peaks in the EIC.…”

Section: Hplc-ms Methods Developmentmentioning

confidence: 99%

“…Particularly in quantitative analysis, multiple reaction monitoring (MRM) in triple quadrupole mass spectrometry (QqQ MS) shows unique selectivity with high sensitivity. Thus, QqQ MS is usually used to detect analytes in complex matrices using MRM with a unique ion transition of the analytes [16,20,22,32]. Although DAD provides the UV spectra of certain compounds identified in a given chromatogram, there are no authentic UV spectra of newly synthesized PDE-5 inhibitors.…”

Section: Introductionmentioning

confidence: 99%

“…In this regard, various spectrometric and chromatographic methods have been adopted to analyze the illegally added drugs in complex matrices [ 3 , 4 , 5 , 9 , 16 , 17 , 18 , 19 , 20 , 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 ]. High-performance liquid chromatography with diode array detection (HPLC–DAD) and liquid chromatography with mass spectrometry (LC–MS) have been previously used to detect PDE-5 inhibitors and their analogs [ 3 , 5 , 7 , 8 , 9 , 10 , 16 , 17 , 20 , 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 , 31 , 32 , 33 , 34 ]. When the standards of PDE-5 inhibitors and their analogs are available, HPLC with a UV spectrometer is a simple method for quantitative analysis [ 11 ].…”

Section: Introductionmentioning

confidence: 99%

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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

et al. 2020

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An accurate and reliable method based on ion trap–time of flight mass spectrometry (IT–TOF MS) was developed for screening phosphodiesterase-5 inhibitors, including sildenafil, vardenafil, and tadalafil, and their analogs in dietary supplements. Various parameters affecting liquid chromatographic separation and IT–TOF detection were investigated, and the optimal conditions were determined. The separation was achieved on a reversed-phase column under gradient elution using acetonitrile and water containing 0.2% acetic acid at a flow rate of 0.2 mL/min. The chromatographic eluents were directly ionized in the IT–TOF system equipped with an electrospray ion source operating in the positive ion mode. The proposed screening method was validated by assessing its linearity, precision, and accuracy. Sequential tandem MS was conducted to obtain structural information of the references, and the fragmentation mechanism of each reference was proposed for providing spectral insight for newly synthesized analogs. Structural information, including accurate masses of both parent and fragment ions, was incorporated into the MSn spectral library. The developed method was successfully applied for screening adulterated dietary supplement samples.

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Section: Hplc-ms Methods Developmentmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

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

et al. 2020

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“…The detection processes of TCM ingredients are complicated and challenging. Several methods are used to determine undeclared adulterants in herbal medicine or food supplements, including the following: LC-PDA [ 12 ], GC-MS [ 13 ], GC-QQQMS [ 14 ], LC-MS [ 15 ], LC-MS/MS [ 12 ], UPLC-TOF/MS [ 16 ], Q-Orbitrap MS [ 17 ], NMR [ 18 ], X-ray powder diffractometry [ 19 ], TLC-image [ 20 ], TLC-SERS [ 21 ], ATR‑IR [ 22 ], and CE-MS [ 23 ]. The applicability of GC‑MS is determined by the volatility and thermal stability of analytes.…”

Section: Introductionmentioning

confidence: 99%

Detection of adulterated drugs in traditional Chinese medicine and dietary supplements using hydrogen as a carrier gas

et al. 2018

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Helium, a minor component of natural gas and radioactive minerals, is most commonly used as a carrier in gas chromatography-mass spectrometry (GC-MS). Its scarcity leads to limited availability and higher costs. In this experiment, hydrogen from a safe source of a hydrogen generator was tested as a substitutive carrier gas for the detection of adulterant in traditional Chinese medicine (TCM) and food supplements by GC-MS analysis. We found that the limits of detection (LODs) of using hydrogen were from 10 to 1000 μg/g. The levels of LODs tested among 170 drugs remain the same whether hydrogen or helium was used as a carrier gas with the exception of 7 drugs—benzbromarone, estradiol benzoate, bezafibrate, mefenamic acid, oxymetholone, piperidenafil and cetilistat. The real sample analysis results using hydrogen were as satisfactory as those using helium. In addition, the retention time was shortened after the chromatographic performance was optimized. In summary, it is worth considering hydrogen as a carrier gas due to its affordable costs, energy efficiency, carbon reduction and chromatographic advantages to detect adulterated drugs in TCM and dietary supplement using GC-MS.

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“…Therefore, the development of a sensitive and accurate analytical method for the simultaneous determination of PDE‐5 inhibitors is very crucial for screening of these drugs in complex matrices such as food and biological samples. There have been several reports in literature for the determination of different PDE‐5 inhibitors using HPLC , GC–MS or GC–MS/MS and LC–MS or LC–MS/MS . These methods have been used for the determinations of sildenafil, tadalafil and vardenafil in pharmaceuticals, biological samples such as hair, urine, plasma and breast milk, environmental samples (waste water and sewage sludge), beverage samples (energy drinks), herbal and dietary supplements.…”

Section: Introductionmentioning

confidence: 99%

Accurate and sensitive determination of sildenafil, tadalafil, vardenafil, and avanafil in illicit erectile dysfunction medications and human urine by LC with quadrupole‐TOF‐MS/MS and their behaviors in simulated gastric conditions

Özbek

Bakırdere

2018

J of Separation Science

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The widespread use of phosphodiesterase‐5 inhibitors has attracted broad attention of counterfeiters to develop illicit erectile products with inaccurate amounts, unknown toxicity, and purity of active ingredients. Correspondingly, intake of these products endangers consumer health and needs to be screened for precautionary actions to reduce this risk. Therefore, in this study, a sensitive and rapid analytical method has been developed for simultaneous determination of selected phosphodiesterase‐5 inhibitors present in illicit erectile medications and human urine. Quantification of the analytes was performed by liquid chromatography coupled with quadrupole‐time‐of‐flight tandem mass spectrometry system. The chromatographic separation was successfully achieved with a run period of 8 min. Low detection limits were obtained in the range of 1.63–9.81 ng/g with relative standard deviations below 7.72% obtained using the replicate measurements of lowest concentration in calibration plots. The analytical performance of the proposed method proved good linearity, low detection limits, good accuracy and precision with high percent recoveries for human urine samples. Developed method was successfully applied to real samples including four different brands of illicit erectile medications. The results obtained revealed the presence of high levels of sildenafil in analyzed samples. The behaviors of selected phosphodiesterase‐5 inhibitors were also studied in simulated gastric conditions.

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Rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography–triple quadrupole mass spectrometry

Cited by 43 publications

References 31 publications

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

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

Detection of adulterated drugs in traditional Chinese medicine and dietary supplements using hydrogen as a carrier gas

Accurate and sensitive determination of sildenafil, tadalafil, vardenafil, and avanafil in illicit erectile dysfunction medications and human urine by LC with quadrupole‐TOF‐MS/MS and their behaviors in simulated gastric conditions

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