Merck
  • Home
  • Search Results
  • Determination of flibanserin and tadalafil in supplements for women sexual desire enhancement using high-performance liquid chromatography with tandem mass spectrometer, diode array detector and charged aerosol detector.

Determination of flibanserin and tadalafil in supplements for women sexual desire enhancement using high-performance liquid chromatography with tandem mass spectrometer, diode array detector and charged aerosol detector.

Journal of pharmaceutical and biomedical analysis (2014-02-18)
Magdalena Poplawska, Agata Blazewicz, Paulina Zolek, Zbigniew Fijalek
ABSTRACT

The new compound - flibanserin - begun to appear as a synthetic adulterant in counterfeit herbal supplements used to stimulate women sexual drive. It was detected in two samples submitted to the Polish National Medicines Institute for analysis. The second sample contained also tadalafil. This study presents the LC method development which enables the determination of flibanserin and tadalafil. It employs three different detectors charged aerosol detector (CAD), diode array detector (DAD) and mass spectrometer (MS). The conditions of the elaborated method were optimized to obtain the highest sensitivity and the best resolution, especially the separation of icariin - the natural compound observed often in supplements for sexual disorders. The validation of the method proved good linearity, good accuracy and precision of the measurements recorded by all three detectors. Additionally, for CAD data, an alternative calculation method using a unified calibration function was presented and evaluated. It seems that this is the way to overcome the problem of non-availability of the reference standard of a target compound. Flibanserin content was quantified using the data of other reference standard (tadalafil). The inaccuracy of proposed indirect determination was found to be ±3%. A statistical evaluation proved that the results obtained with all detection modes and the results calculated using a unified calibration were not significantly different (p>0.05).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, for residue analysis, JIS 5000
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Methanol, SAJ special grade
Sigma-Aldrich
Methanol, suitable for HPLC
Sigma-Aldrich
Methanol, NMR reference standard
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 0.1 % (v/v) formic acid, 5 % (v/v) water, suitable for HPLC
Sigma-Aldrich
Methanol, JIS 1000, ≥99.8%, for residue analysis
Sigma-Aldrich
Methanol, ≥99.8%, suitable for absorption spectrum analysis
Sigma-Aldrich
Methanol, ≥99.8%, for chromatography
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, for residue analysis
Sigma-Aldrich
Ammonium formate, SAJ first grade, ≥95.0%
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)