Quantitation of tadalafil in human plasma by liquid chromatography–tandem mass spectrometry with electrospray ionization

Ramakrishna, N. V. S.; Vishwottam, K.N.; Puran, S.; Koteshwara, M.; Manoj, S.; Santosh, M.; Chidambara, J.; Wishu, S.; Sumatha, B.

doi:10.1016/j.jchromb.2004.06.026

Cited by 46 publications

(61 citation statements)

References 10 publications

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“…Recently, several groups have reported HPLC-MS/MS assays using 2 or 3 mm i.d. columns, after either liquid-liquid extraction or solid-phase extraction (SPE), to determine drug compounds in plasma samples at low concentrations [4][5][6][7][8][9][10][11][12][13][14][15]. With all of these published methods, the lower limit of quantification of the drug in plasma was <1 ng ml −1 and the on-column mass sensitivity was ≤5 pg.…”

Section: Introductionmentioning

confidence: 99%

Application of microbore HPLC in combination with tandem MS for the quantification of rosuvastatin in human plasma

Oudhoff

Sangster

Thomas

et al. 2006

Journal of Chromatography B

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Section: Introductionmentioning

confidence: 99%

Application of microbore HPLC in combination with tandem MS for the quantification of rosuvastatin in human plasma

Oudhoff

Sangster

Thomas

et al. 2006

Journal of Chromatography B

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“…The lower limits of detection under the scan mode were 0.05 ng for vardenaˆl (as HCl･ 3H 2 O salt), 0.1 ng for both sildenaˆl (as citrate salt) and hydroxyhomosildenaˆl and 0.25 ng for tadalaˆl in terms of on-column amount (S/N＞ 5). Under the selected ion monitoring of their protonated molecules, the sensitivities were enhanced about 10 times, which was comparable to those required to analyze biological samples 12,20,21) . Quantitative analysis of the compounds was carried out using HPLC (UV 230 nm).…”

Section: Resultsmentioning

confidence: 94%

Chemical Profile of Sildenafil and Related Compounds

Inoue

Kanamori

Kuwayama

et al. 2008

Jpn. J. Forensic. Sci. Tech.

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Sildenaˆland related compounds, vardenaˆl, tadalaˆl and hydroxyhomosildenaˆl, in dietary supplements were characterized using thin layer chromatography (TLC), infrared (IR) spectroscopy, gas chromatography/mass spectrometry (GC/MS), high performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). TLC with DragendorŠ reagent gave a lower detection limit than 1 mg for all 4 compounds. IR spectra of the compounds were so characteristic as to discriminate one from another easily. After TMS derivatization, all the peaks of these compounds appeared and well-separated on the GC/MS chromatograms at a high column temperature (320°C), although hydroxyhomosildenaˆl was not detected without derivatization. In HPLC and LC/ MS analyses, an ODS column with a mobile phase composed of a mixture of 20 mM ammonium acetate (pH 5.0) and methanol (4060) allowed separation of the 4 compounds. Simple electrospray-ionization mass spectra with only protonated molecules were obtained except for tadalaˆl, which was cleaved easier than the other compounds, so cone voltage should be lower for tadalaˆl. Quantitative analysis of the 4 compounds was carried out using HPLC (UV at 230 nm). The lower limit of detection for each compound was 50 ng/ml at a 10-ml injection volume (0.5 ng on the column, S/N＞3). A calibration curve was linear in the range of 0.01 1.0 mg/ml for each compound (r 2 ＞0.997). Our methods were applied to casework samples (conˆscated tablets), and disclosed that those tablets contained varying amounts of sildenaˆl and/or tadalaˆl and were counterfeit products.

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“…The linearity of the method was evaluated based a calibration curve in the range of 5 to 1,000 ng/mL, which was the expected concentration range after a single oral dose of tadalafil 20 mg. [12] Each calibration curve was constructed based on the least squares linear regression of the tadalafil to IS peak area ratio versus the nominal analyte concentrations with a weighting factor of 1/x. Deviations of these back-calculated concentrations from the spiked concentrations were set within ±15% (±20% for the LLOQ) of the theoretical value.…”

Section: Linearity and Lower Limit Of Quantificationmentioning

confidence: 99%

“…[11] In recent pharmacokinetic studies, LC-tandem mass spectrometry (LC-MS/MS) has primarily been used for measuring tadalafil in plasma because of its high sensitivity and selectivity. [12][13][14][15][16][17][18][19] Proença et al published a validated ultra-performance liquid chromatography (UPLC)-MS/ MS method for the analysis of sildenafil, vardenafil, and tadalafil in postmortem blood samples. [17] Lee et al also reported an LC-MS/MS method for the determination of five ED drugs and their selected metabolites in hair to monitor abuse of mirodenafil, sildenafil, tadalafil, udenafil and vardenafil.…”

Section: Introductionmentioning

confidence: 99%

Validated UPLC-MS/MS method for the determination of tadalafil in human plasma and its application to a pharmacokinetic study

Kim

Nam

Kwon

et al. 2017

Transl Clin Pharmacol

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A simple, rapid, and reliable UPLC-MS/MS method was developed and validated for the determination of tadalafil in human plasma. The plasma samples were deproteinized with acetonitrile. Chromatographic separation was performed on a Shiseido C18 (100 × 2.1 mm, 2.7 μm) column with isocratic elution using 2.0 mM ammonium acetate and acetonitrile (55:45, v/v) with 0.1% formic acid at a flow rate of 0.7 mL/min. The total run time was 1 min per sample. The quantitative analysis was performed using multiple reaction monitoring at transition of m/z 390.4 → 268.3 for tadalafil and m/z 475.3 → 283.3 for sildenafil as an internal standard. The method was fully validated over a concentration range of 5-1,000 ng/mL with a lower quantification limit of 5 ng/mL. Intra-and inter-day precision (relative standard deviation, %RSD) were within 8.4% and accuracy (relative error, %RE) was lower than -3.2%. The developed and validated method was successfully applied to a pharmacokinetic study of tadalafil (20 mg) in Korean healthy male subjects (n = 12).

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Quantitation of tadalafil in human plasma by liquid chromatography–tandem mass spectrometry with electrospray ionization

Cited by 46 publications

References 10 publications

Application of microbore HPLC in combination with tandem MS for the quantification of rosuvastatin in human plasma

Application of microbore HPLC in combination with tandem MS for the quantification of rosuvastatin in human plasma

Chemical Profile of Sildenafil and Related Compounds

Validated UPLC-MS/MS method for the determination of tadalafil in human plasma and its application to a pharmacokinetic study

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