Home >Current Issue
Volume: 9, Issue: 7, July, 2019
A validated LC-ESI-MS/MS method for the quantification of Selegiline HCl in bulk and pharmaceutical formulationAuthor Affiliations
Selegiline HCl is an irreversible MAO-B inhibitor used to reduce symptoms in early-stage Parkinson’s disease. It is used as an adjunct to drugs, such as L Dopamine (L-DOPA). The present study is designed to develop and validate a rapid, sensitive, and straightforward separation method with Electrospray ionization and triple quadrupole mass analyzer for the quantification of Selegiline HCl in bulk and pharmaceutical formulation. Zorbax C18 column (50 mm × 4.6 mm i.d, 5 μ particle size) was used for the separation of analyte and internal standard. The samples were eluted using 0.1% Formic acid in water and Methanol (40:60%v/v) which is delivered at 0.5 ml/minute flow rate, with a chromatographic runtime of 5 minutes. The eluents were monitored using a tandem mass spectrometer equipped with an electrospray ionization in positive mode and a triple quadrupole mass analyzer. The detection was carried out in multiple reaction-monitoring mode by quantifying the m/z 188.05→91.10 ion transition pair; with collision energy −29.0 V for Selegiline HCl. Linearity was achieved over the concentration range 3.5–6.5 ng/ml for the developed method. The limit of detection and limit of quantification were found to be 0.2 and 0.5 ng/ml, respectively. The correlation coefficient (r2) value was ≥0.9985 for Selegiline HCl. This method offers a sensitive quantification of Selegiline HCl in the pharmaceutical formulation.
Copyright: The Author(s). This is an open access article distributed under the Creative Commons Attribution Non-Commercial License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Danafar H. Simple and sensitive high-performance liquid chromatographic (HPLC) method for the determination of the selegiline in human plasma. Cognet Med, 2016; 3:1179244. https://doi.org/10.1080/2331205X.2016.1179244
Heinonen EH, Anttila MI, Lammintausta RA. Pharmacokinetic aspects of L-deprenyl (selegiline) and its metabolites. Clin Pharmacol Ther, 1994; 56:742-9. https://doi.org/10.1038/clpt.1994.204
Kalaskar RC, Nagras MA. Stability Indicating RP-HPLC Method for Selegiline hydrochloride in pharmaceutical formulations. Asian J Pharm Res Dev, 2014; 2:5-13.
Katagi M, Tatsuno M, Miki A, Nishikawa M, Nakajima K, Tsuchihashi H. Simultaneous determination of selegiline-N-oxide, a new indicator for selegiline administration, and other metabolites in urine by high-performance liquid chromatography-electrospray ionization mass spectrometry. J Chromatogr B, 2001; 759:125-33. https://doi.org/10.1016/S0378-4347(01)00213-4
Knoll J. The pharmacological profile of (-) deprenyl (Selegiline) and its relevance for humans: a personal view. Pharmacol Toxicol, 1992; 70:317-21. https://doi.org/10.1111/j.1600-0773.1992.tb00480.x
La Croix R, Pianezzola E, Strolin Benedetti M. Sensitive high-performance liquid chromatographic method for the determination of the three main metabolites of selegiline (L-deprenyl) in human plasma. J Chromatogr B, 1994; 656:251-8. https://doi.org/10.1016/0378-4347(94)00039-5
Magyar K. The pharmacology of selegiline. Int Rev Neurobiol, 2011; 100:65-84. https://doi.org/10.1016/B978-0-12-386467-3.00004-2
Nishida K, Itoh S, Inoue N, Kudo K, Ikeda N. High-performance liquid chromatographic-mass spectrometric determination of methamphetamine and amphetamine enantiomers, desmethylselegiline and Selegiline in hair samples of long-term methamphetamine abusers or Selegiline users. J Anal Toxicol, 2006; 30:233-7. https://doi.org/10.1093/jat/30.4.232
Slawson MH, Taccogno JL, Foltz RL, Moody DE. Quantitative analysis of selegiline and three metabolites (N- desmethylselegiline, methamphetamine, and amphetamine) in human plasma by high-performance liquid chromatography- atmospheric pressure chemical ionization-tandem mass spectrometry. J Anal Toxicol, 2002; 26:430-7. https://doi.org/10.1093/jat/26.7.430
Tzanavaras PD, Themelis DG, Zotou A, Stratis J, Karlberg B. Optimization and validation of a dissolution test for selegiline hydrochloride tablets by a novel rapid HPLC assay using a monolithic stationary phase. J Pharm Biomed Anal, 2008; 46:670-5. https://doi.org/10.1016/j.jpba.2007.11.039
ICH Topic Q2 (R1). Validation of analytical procedure: text and methodology Q2(R1). In International Conference on Harmonisation of Technical Requirements for registration of Pharmaceuticals for human use, 2005.