Skip to main content

Butyl-based reversed-phase high-performance liquid chromatography and silica normal-phase high-performance thin-layer chromatography methods for the determination of palonosetron in the presence of degradation products and dosage form additives

Abstract

Stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) and normal-phase high-performance thin-layer chromatography (NP-HPTLC) methods have been developed for the determination of palonosetron which is a potent antiemetic drug used with chemotherapy. Forced degradation studies were performed on palonosetron to study its stability behavior. The drug was subjected to acid, base, neutral hydrolysis, oxidation, thermal and photolytic conditions. Mass analysis has been performed to elucidate the oxidative degradants by Advion compact mass spectrometer. HPLC separation was achieved on PerfectChrom 100 C4 (250 × 4.6 mm, 5 μm particle size) column using buffer (20 mM dipotassium hydrogen orthophosphate, adjusted with phosphoric acid to pH 2.5):acetonitrile:methanol (60:30:10, v/v) as the mobile phase with isocratic mode at a flow rate of 1 mL/min using photodiode array detector (PAD) at 210 nm. The method showed adequate sensitivity concerning linearity, accuracy and precision over the range of 0.1–10 μg/mL. Limit of detection (LOD) and limit of quantification (LOQ) were determined to be 0.03 μg/mL and 0.09 μg/mL, respectively. HPTLC separation was carried out on aluminum plates pre-coated with silica gel 60 F254 using methanol:ammonia (10:0.5, v/v) as the mobile phase. CAMAG scanner was operated at 254 nm for the densitometric measurement in the absorbance mode. A polynomial relationship was constructed in concentration range of 0.1–2 μg/band, with LOD and LOQ 0.02 μg/band and 0.06 μg/band, respectively. The cited chromatographic methods were successfully applied to the determination of palonosetron in the presence of its degradation products and additives in the commercially available vials. Method validation was performed as per the ICH guidelines confirming methods robustness to be used in quality control laboratories. Statistical comparisons have been performed between the results of the cited chromatographic methods and those of the official one using Student’s t test and F test values at 95% confidence interval level, revealing good accuracy and precision.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7

References

  1. Klick S, Muijselaar PG, Waterval J, Eichinger T, Korn C, Gerding TK, Debets AJ, van de Griend CS, van den Beld C, Somsen GW, Jong GJD (2005) Pharm. Technol 29:48–66

    Google Scholar 

  2. FDA Guidance for Industry: Impurities in Drug Substances, Food and Drug Administration, Rockville, MD, 2005

  3. Patel BMRD, Prajapati PN, Agrawal YK (2014) J. Pharm. Anal 4:159–165

    Article  Google Scholar 

  4. Kumar V, Bharadwaj R, Gupta G, Kumar S (2015) Pharm Chem J 2:30–40

    CAS  Google Scholar 

  5. Kastner M (2000) Protein liquid chromatography, vol 61. Elsevier Science, Amsterdam

    Google Scholar 

  6. M. C. García-Alvarez-Coque, J. J. Baeza-Baeza, G. Ramis-Ramos, Reversed phase liquid chromatography Analytical Separation Science: Wiley-VCH 2015. 159–198

  7. A. De Leon, Proc (Bayl Univ Med Cent) 19 (2006) 413–416

  8. Brayfield A (2018) Martindale: the complete drug reference, 39th edn. Pharmaceutical Press, London

    Google Scholar 

  9. United States Pharmacopeia, USP 41, NF 36, Rockville, MD, 2018

  10. Murthy MV, Srinivas K, Kumar R, Mukkanti K (2011) J Pharm Biomed Anal 56:429–435

    Article  Google Scholar 

  11. Parekh D, Patel CJ, Patel MM (2018) World J Pharm Res 7:723–736

    Google Scholar 

  12. Damle MC, Agrawal AA (2015) Am J PharmTech Res 5:275–286

    Google Scholar 

  13. Jain PS, Chavan RS, Bari PR, Patil SS, Surana SJ, Adv J (2015) Drug Deliv 2

  14. Pathi PJ, Raju NA (2012) Asian J Pharm Technol 2:77–79

    Google Scholar 

  15. Inturi S, Inturi R, Venkatesh G (2011) Pharm Sin 2:223–234

    CAS  Google Scholar 

  16. Li P, Ma P, Wang Y, Tong W, Wang J, Wu C, Liu L (2012) J Chromatogr B 895-896:10–16

    CAS  Article  Google Scholar 

  17. Wang Y, Wang Y, Zhang P, Lu Z, Gu Y, Ou N (2011) Determination of palonosetron in human urine by LC-MS/MS. Bioanalysis 3:1337–1342

    CAS  Article  Google Scholar 

  18. Yang S, Qin F, Wang D, Li N, Li F, Xiong Z (2012) Determination of palonosetron in human plasma by ultra performance liquid chromatography-tandem mass spectrometry and its application to a pharmacokinetic study. J Pharm Biomed Anal 57:13–18

    Article  Google Scholar 

  19. Ding L, Chen Y, Yang L, Wen A (2007) Determination of palonosetron in human plasma by liquid chromatography-electrospray ionization-mass spectrometry. J Pharm Biomed Anal 44:575–580

    CAS  Article  Google Scholar 

  20. Zhang W, Feng F, Le W, Wang H, Zhu L (2008) Chromatographia 68:193–199

    CAS  Article  Google Scholar 

  21. Tian K, Chen H, Tang J, Chen X, Hu Z (2006) Enantioseparation of palonosetron hydrochloride by micellar electrokinetic chromatography with sodium cholate as chiral selector. J Chromatogr A 1132:333–336

    CAS  Article  Google Scholar 

  22. Radhakrishnanand P, Subba Rao DV, Himabindu V (2008) Chromatographia 69:369–373

    Article  Google Scholar 

  23. Xiao-rong Y, Min S, Tai-jun H (2008) Chin. J. New Drugs 10

  24. Parambi DGT, Mathew SM, Ganesan V (2011) Int J Chem Sci 4:1619–1624

    Google Scholar 

  25. ICH, Stability testing of new drug substances and products, ICH Harmonised Tripartite Guideline Q1A (R2), Vol. 4, Geneva, 2003, 1–24

  26. ICH. Q2 (R1): Validation of analytical procedures: text and methodology. in International Conference on Harmonization, Geneva, 2005

  27. Moffat A, Osselton M, Widdop B (2011) Clarke’s analysis of drugs and poisons, 4th edn. Pharmaceutical Press, London

    Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Dalia Abdelrazeq Elshabasy.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Tantawy, M.A., Alweshahy, S., Elshabasy, D.A. et al. Butyl-based reversed-phase high-performance liquid chromatography and silica normal-phase high-performance thin-layer chromatography methods for the determination of palonosetron in the presence of degradation products and dosage form additives. JPC-J Planar Chromat 33, 149–160 (2020). https://doi.org/10.1007/s00764-020-00014-3

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00764-020-00014-3

Keywords

  • Butyl-based reversed-phase high-performance liquid chromatography
  • Normal-phase high-performance thin-layer chromatography
  • Palonosetron
  • Forced degradation
  • Method validation