Application of high-performance liquid chromatography with charged aerosol detection for universal quantitation of undeclared phosphodiesterase-5 inhibitors in herbal dietary supplements

Journal of Pharmaceutical and Biomedical Analysis

Volumn 84, Issue , 2013, Pages 232-243

  Poplawska, Magdalena ^a,b   Blazewicz, Agata ^a   Bukowinska, Kinga ^b   Fijalek, Zbigniew ^a,b  

^a NATIONAL MEDICINES INSTITUTE   (Poland)

^b MEDICAL UNIVERSITY OF WARSAW   (Poland)

Author keywords

Adulteration; Charged aerosol detector; Counterfeit dietary supplement; PDE 5 inhibitor; Universal calibration

Indexed keywords

HERBACEOUS AGENT; PHOSPHODIESTERASE V INHIBITOR; SILDENAFIL; TADALAFIL;

ANALYTIC METHOD; ANALYTICAL EQUIPMENT; ARTICLE; CALIBRATION; CHARGED AEROSOL DETECTOR; DIET SUPPLEMENTATION; ELECTROSPRAY; HIGH PERFORMANCE LIQUID CHROMATOGRAPHY; LIMIT OF DETECTION; LIMIT OF QUANTITATION; PRIORITY JOURNAL; QUANTITATIVE ANALYSIS; STANDARD; TIME OF FLIGHT MASS SPECTROMETRY;

ADULTERATION; CHARGED AEROSOL DETECTOR; COUNTERFEIT DIETARY SUPPLEMENT; PDE-5 INHIBITOR; UNIVERSAL CALIBRATION;

AEROSOLS; CHROMATOGRAPHY, HIGH PRESSURE LIQUID; DIETARY SUPPLEMENTS; DRUG CONTAMINATION; HERBAL MEDICINE; PHARMACEUTICAL SOLUTIONS; PHOSPHODIESTERASE 5 INHIBITORS; PLANT PREPARATIONS; POWDERS; REFERENCE STANDARDS; SPECTROMETRY, MASS, ELECTROSPRAY IONIZATION; SUBSTANCE ABUSE DETECTION;

EID: 84880341377     PISSN: 07317085     EISSN: 1873264X     Source Type: Journal    
DOI: 10.1016/j.jpba.2013.06.018     Document Type: Article

References (35)

1. Petroczi A., Taylor G., Naughton G.P. Mission impossible? Regulatory and enforcement issues to ensure safety of dietary supplements. Food Chem. Toxicol. 2011, 49:393-402.
2. Venhuis B.J., Blok-Tip L., de Kaste D. Designer drugs in herbal aphrodisiacs. For. Sci. Int. 2008, 177:e25-e27.
3. Venhuis B.J., de Kaste D. Towards a decade of detecting new analogues of sildenafil, tadalafil and vardenafil in food supplements: a history, analytical aspects and health risks, J. Pharm. Biomed. Anal. 2012, 69:196-208.
4. Song F., El-Demerdash A., Lee S.J.S.H. 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. J. Pharm. Biomed. Anal. 2012, 70:40-46.
5. Bogusz M.J., Hassan H., Al-Enazi E., Ibrahim Z., Al-Tufail M. Application of LC-ESI-MS-MS for detection of synthetic adulterants in herbal remedies. J. Pharm. Biomed. Anal. 2006, 41:554-564.
6. Zou P., Oh S.S.Y., Hou P., Low M.Y., Koh H.L. Simultaneous determination of synthetic phosphodiesterase-5 inhibitors found in a dietary supplement and pre-mixed bulk powders for dietary supplements using high-performance liquid chromatography with diode array detection and liquid chromatography-electrospray ionization tandem mass spectrometry. J. Chromatogr. A 2006, 1104:113-122.
7. Zhang Y., Huang Z., Ding L., Yan H., Wang M., Zhu S. Simultaneous determination of yohimbine, sildenafil, vardenafil and tadalafil in dietary supplements using high-performance liquid chromatography-tandem mass spectrometry. J. Sep. Sci. 2010, 33:2109-2114.
8. Nieto A., Peschka M., Borrull F., Pocurull E., Marcé R.M., Knepper T.P. Phosphodiesterase Type V inhibitors: occurrence and fate in wastewater. Water Res. 2010, 44:1607-1615.
9. Ku H.Y., Shon J.H., Liu K.H., Shin J.G., Bae S.K. Liquid chromatography/tandem mass spectrometry method for the simultaneous determination of vardenafil and its major metabolite, N-desethylvardenafil, in human plasma: application to a pharmacokinetic study. J. Chromatogr. B: Analyt. Technol. Biomed. Life Sci. 2009, 877:95-100.
10. Lake S.T., Altman P.M., Vaisman J., Addison R.S. Validated LC-MS/MS assay for the quantitative determination of vardenafil in human plasma and its application to a pharmacokinetic study. Biomed. Chromatogr. 2010, 24:846-851.
11. Bartošová Z., Jirovský D., Horna A. High-performance liquid chromatographic method with amperometric detection employing boron-doped diamond electrode for the determination of sildenafil, vardenafil and their main metabolites in plasma. J. Chromatogr. A 2011, 1218:7996-8001.
12. Balayssac S., Gilard V., Zedde Ch., Martino R., Malet-Martino M. Analysis of herbal dietary supplements for sexual performance enhancement: first characterization of propoxyphenyl-thiohydroxyhomosildenafil and identification of sildenafil, thiosildenafil, phentolamine and tetrahydropalmatine as adulterants. J. Pharm. Biomed. Anal. 2012, 63:135-150.
13. Sacré P.Y., Deconinck E., Chiap P., Crommen J., Mansion F., Rozet E., Courselle P., De Beer J.O. Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines. J. Chromatogr. A 2011, 1218:6439-6447.
14. De Orsi D., Pellegrini M., Marchei E., Nebuloni P., Gallinella B., Scaravelli G., Martufi A., Gagliardi L., Pichini S. High performance liquid chromatography-diode array and electrospray-mass spectrometry analysis of vardenafil, sildenafil, tadalafil, testosterone and local anesthetics in cosmetic creams sold on the Internet web sites. J. Pharm. Biomed. Anal. 2009, 50:362-369.
15. Balayssac S., Trefi S., Gilard V., Malet-Martino M., Martino R., Delsuc M.A. 2D and 3D DOSY 1H NMR, a useful tool for analysis of complex mixtures: application to herbal drugs or dietary supplements for erectile dysfunction. J. Pharm. Biomed. Anal. 2009, 50:602-612.
16. Gratz S.R., Flurer C.L., Wolnik K.A. Analysis of undeclared synthetic phosphodiesterase-5 inhibitors in dietary supplements and herbal matrices by LC-ESI-MS and LC-UV. J. Pharm. Biomed. Anal. 2004, 36:525-533.
17. Holzgrabe U., Malet-Martino M. Analytical challenges in drug counterfeiting and falsification - the NMR approach. J. Pharm. Biomed. Anal. 2011, 55:679-687.
18. Kesting J.R., Huang J., Sørensen D. Identification of adulterants in a Chinese herbal medicine by LC-HRMS and LC-MS-SPE/NMR and comparative in vivo study with standards in a hypertensive rat model. J. Pharm. Biomed. Anal. 2010, 51:705-711.
19. Novoa-Carballal R., Fernandez-Megia E., Jimenez C., Riguera R. NMR methods for unravelling the spectra of complex mixtures. Nat. Prod. Rep. 2011, 28:78-98.
20. Dixon R.W., Peterson D.S. Development and testing of a detection method for liquid chromatography based on aerosol charging. Anal. Chem. 2002, 74:2930-2937.
21. Vehovec T., Obreza A. Review of operating principle and applications of the charged aerosol detector. J. Chromatogr. A 2010, 1217:1549-1556.
22. Lane S., Boughtflower B., Mutton I., Paterson C., Farrant D., Taylor N., Blaxill Z., Carmody C., Borman P. Toward single-calibrant quantification in HPLC. A comparison of three detection strategies: evaporative light scattering, chemiluminescent nitrogen, and proton NMR. Anal. Chem. 2005, 77:4354-4365.
23. Vervoort N., Daemen D., Török G. Performance evaluation of evaporative light scattering detection and charged aerosol detection in reversed phase liquid chromatography. J. Chromatogr. A 2008, 1189:92-100.
24. Gamache P.H., McCarthy R.S., Freeto S.M., Asa D.J., Woodcock M.J., Laws K., Cole R.O. HPLC analysis of nonvolatile analytes using charged aerosol detection. LC-GC North Am. 2005, 23:150-161.
25. Górecki T., Lynen F., Szucs R., Sandra P. Universal response in liquid chromatography using charged aerosol detection. Anal. Chem. 2006, 78:3186-3192.
26. Schiesel S., Lämmerhofer M., Lindner W. Comprehensive impurity profiling of nutritional infusion solutions by multidimensional off-line reversed-phase liquid chromatography×hydrophilic interaction chromatography-ion trap mass-spectrometry and charged aerosol detection with universal calibration. J. Chromatogr. A 2012, 1259:100-110.
27. Stojanovic A., Lämmerhofer M., Kogelnig D., Schiesel S., Sturm M., Galanski M., Krachler R., Keppler B.K., Lindner W. Analysis of quaternary ammonium and phosphonium ionic liquids by reversed-phase high-performance liquid chromatography with charged aerosol detection and unified calibration. J. Chromatogr. A 2008, 1209:179-187.
28. Holzgrabe U., Nap C.J., Kunz N., Almeling S. Identification and control of impurities in streptomycin sulfate by high-performance liquid chromatography coupled with mass detection and corona charged-aerosol detection. J. Pharm. Biomed. Anal. 2011, 56:271-279.
29. Sun P., Wang X., Alquier L., Maryanoff C.A. Determination of relative response factors of impurities in paclitaxel with high performance liquid chromatography equipped with ultraviolet and charged aerosol detectors. J. Chromatogr. A 2008, 1177:87-91.
30. Loughlin J., Phan H., Wan M., Guo S., May K., Lin B. Evaluation of charged aerosol detection (CAD) as a complementary technique for high-throughput LC-MS-UV-ELSD analysis of drug discovery screening libraries. Am. Lab. 2007, 39:24-27.
31. Hutchinson J.P., Li J., Farrell W., Groeber E., Szucs R., Dicinoski G., Haddad P.R. Universal response model for a corona charged aerosol detector. J. Chromatogr. A 2010, 1217:7418-7427.
32. Gratz S.R., Zeller M., Mincey D.W., Flurer C.L. Structural characterization of sulfoaildenafil, an analog of sildenafil. J. Pharm. Biomed. Anal. 2009, 50:228-231.
33. Blazewicz A., Fijalek Z., Warowna-Grzeskiewicz M., Jadach M. Determination of atracurium, cisatracurium and mivacurium with their impurities in pharmaceutical preparations by liquid chromatography with charged aerosol detection. J. Chromatogr. A 2010, 1217:1266-1272.
34. International Conference on Harmonization (ICH), Topic Q2 (R1): Validation of Analytical Procedures: Text and Methodology, Geneva 2005, http://www.emea.europa.eu/pdfs/human/ich/038195en.pdf.
35. RIVM Report 370030001/2007. Recent developments in counterfeits and imitations of Viagra, Cialis and Levitra A 2005-2006 update.