Screening for multiple phosphodiesterase type 5 inhibitor drugs in dietary supplement materials by flow injection mass spectrometry and their quantification by liquid chromatography tandem mass spectrometry

Song, Fenhong; El-Demerdash, Aref; Lee, Shwn-Ji Susie H.

doi:10.1016/j.jpba.2012.05.017

Cited by 39 publications

(22 citation statements)

References 21 publications

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“…ACN and MeOH have been widely used as organic solvent in PDE-5 inhibitors analysis using LCMS and LC-MS/MS [3,[13][14][15]21]. Additionally, ammonium formate and acetic acid (with formic acid or not) were selected as a solvent modifier [3,14,15,21,22].…”

Section: Optimization Of Lc-ms/ms Measurement Conditionsmentioning

confidence: 99%

“…Additionally, ammonium formate and acetic acid (with formic acid or not) were selected as a solvent modifier [3,14,15,21,22]. According to previous research, MeOH was not good for separation between sildenafil and vardenafil [14,20], and formic acid was not suitable for analysis of the compounds having amino groups such as sildenafil, homosildenafil, and hydroxyhomosildenafil [18].…”

Section: Optimization Of Lc-ms/ms Measurement Conditionsmentioning

confidence: 99%

“…Meanwhile, several authors reported the screening and confirmation method of synthetic PDE-5 inhibitors in dietary supplements [9][10][11][12][13][14][15][16]. The ultra-high-performance liquid chromatography (UHPLC)-UV method for nine ED drugs and some of their analogues was developed and validated [9].…”

Section: Introductionmentioning

confidence: 99%

“…Song et al presented the flow injection tandem mass spectrometry method (FI-MS/MS) to identify PDE-5 inhibitors and their analogues [15]. A gas chromatography-mass spectrometry (GC-MS) method was used to analyze thioketone analogues of sildenafil [16].…”

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

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

Lee

Han

et al. 2013

Journal of Pharmaceutical and Biomedical Analysis

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Section: Optimization Of Lc-ms/ms Measurement Conditionsmentioning

confidence: 99%

Section: Optimization Of Lc-ms/ms Measurement Conditionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

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

Lee

Han

et al. 2013

Journal of Pharmaceutical and Biomedical Analysis

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“…There are several methods described in the literature for SILC API determination or dosage forms by various techniques. Most of these methods are based on the high-performance liquid chromatography (HPLC) or ultra-performance liquid chromatography (UPLC) using UV-Vis or mass detectors, however, they require several pieces of expensive reagents/equipments (Gratz, Flurer, Wolnik, 2004;De Orsi et al, 2009;Song, El-Demerdash, Lee, 2012;Damiano et al, 2014;Fejos et al, 2014).…”

Section: Introductionmentioning

confidence: 99%

Development and validation of alternative methods by non-aqueous acid-base titration and derivative ultraviolet spectrophotometry for quantification of sildenafil in raw material and tablets

Silva

Toledo

Vianna-Soares

2017

Braz. J. Pharm. Sci.

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Sildenafil citrate (SILC) is a potent phosphodiesterase-5 inhibitor used for erectile dysfunction and pulmonary hypertension. This study shows two simple, fast and alternative analytical methods for SILC determination by non-aqueous titration and by derivative ultraviolet spectrophotometry (DUS) in active pharmaceutical ingredient and/or dosage forms. The quantitation method of SILC active pharmaceutical ingredient by non-aqueous acid-base titration was developed using methanol as solvent and 0.1 mol/L of perchloric acid in acetic acid as titrant. The endpoint was potentiometrically detected. The non-aqueous titration method shows satisfactory repeatability and intermediate precision (RSD 0.70-1.09%). The neutralization reaction occurred in the stoichiometric ratio 1:1 in methanol. The determination of SILC active pharmaceutical ingredient or dosage forms by DUS was developed in the linear range from 10 to 40 µg/mL, in 0.01 mol/L HCl, using the first order zero-peak method at λ 256 nm. The DUS method shows selectivity toward tablets excipients, appropriate linearity (R 2 0.9996), trueness (recovery range 98.86-99.30%), repeatability and intermediate precision in three concentration levels (RSD 1.17-1.28%; 1.29-1.71%, respectively). Therefore, the methods developed are excellent alternatives to sophisticated instrumental methods and can be easily applied in any pharmaceutical laboratory routine due to simple and fast executions.Uniterms: Sildenafil citrate. Vasodilator. Derivative ultraviolet spectrophotometry. Non-aqueous acidbase titrimetry. Sildenafil citrate/quality control.

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Validated spectrofluorimetric method for determination of two phosphodiesterase inhibitors tadalafil and vardenafil in pharmaceutical preparations and spiked human plasma

et al. 2015

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A valid, sensitive and rapid spectrofluorimetric method has been developed and validated for determination of both tadalafil (TAD) and vardenafil (VAR) either in their pure form, in their tablet dosage forms or spiked in human plasma. This method is based on measurement of the native fluorescence of both drugs in acetonitrile at λem 330 and 470 nm after excitation at 280 and 275 nm for tadalafil and vardenafil, respectively. Linear relationships were obtained over the concentration range 4-40 and 10-250 ng/mL with a minimum detection of 1 and 3 ng/mL for tadalafil and vardenafil, respectively. Various experimental parameters affecting the fluorescence intensity were carefully studied and optimized. The developed method was applied successfully for the determination of tadalafil and vardenafil in bulk drugs and tablet dosage forms. Moreover, the high sensitivity of the proposed method permitted their determination in spiked human plasma. The developed method was validated in terms of specificity, linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), precision and accuracy. The mean recoveries of the analytes in pharmaceutical preparations were in agreement with those obtained from the comparison methods, as revealed by statistical analysis of the obtained results using Student's t-test and the variance ratio F-test.

show abstract

Screening for multiple phosphodiesterase type 5 inhibitor drugs in dietary supplement materials by flow injection mass spectrometry and their quantification by liquid chromatography tandem mass spectrometry

Cited by 39 publications

References 21 publications

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

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

Development and validation of alternative methods by non-aqueous acid-base titration and derivative ultraviolet spectrophotometry for quantification of sildenafil in raw material and tablets

Validated spectrofluorimetric method for determination of two phosphodiesterase inhibitors tadalafil and vardenafil in pharmaceutical preparations and spiked human plasma

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