Araştırma Makalesi
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Farmasötik Şekillerde Galantamin Miktarının Belirlenmesi İçin Alternatif Analitik Yöntemler

Yıl 2022, , 58 - 64, 31.08.2022
https://doi.org/10.33713/egetbd.1161168

Öz

Amaç: Galantaminin yığın halinde ve farmasötik dozaj formunda miktar tayini için, yeni seçici, hızlı, kesin ve doğru spektrofotometrik ve kromatografik prosedürler geliştirildi ve doğrulandı.

Gereç ve Yöntem: Kromatografik ayırma, bir Agilent Extend C18 (250x4.6 mm, 5 um) kolonu üzerinde gerçekleştirilmiştir. %0,1 TFA içeren ultra saf su ve %0,1 TFA içeren asetonitril (85/15, v/v) 1.0 mL/dk akış hızında mobil faz olarak kullanıldı. Eluent tespiti, bir UV detektörü kullanılarak 288 nm dalga boyunda gerçekleştirilmiştir. Galantamin ise 288 nm dalga boyunda çözeltilerin absorbansı ölçülerek spektrofotometrik teknikle belirlendi.

Bulgular: Galantamin için Lambert−Beer grafikleri, 5-30 μg/mL konsantrasyon aralığında doğrusal ilişkiler gösterdi. Her iki teknik de Uluslararası Uyumlaştırma Konferansı (ICH) standartlarını karşılamak için istatistiksel olarak değerlendirilmiş ve doğrulanmıştır ve sonuçlar, spektrofotometrik ve sıvı kromatografik yöntemlerin doğrusal, hassas, doğru, sağlam ve RSD değerlerinin %1,00'dan düşük olduğunu göstermiştir. ve geri kazanım yüzdesi standart sınırlar içindeydi (%98-102). Daha sonra bu analitik yöntemlerin istatistiksel bir karşılaştırması yapıldı. Her iki yöntemin sonuçları da %95 güven aralığında (p<0,05) birbirlerine göre farklılık göstermedi ve istatistiksel olarak anlamlı değildi.

Sonuç: Geliştirilen analitik yöntemlerin doğru, oldukça etkili, güvenilir, hızlı, basit olduğu belirlendi ve farmasötik dozaj formunun yanı sıra yığın halindeki galantaminin rutin analizi için başarıyla kullanılabilir. Kalite kontrol analizi ve temizlik doğrulaması sırasında numune analizi için bile kullanılabilirler.

Kaynakça

  • Ferri, C.P., et al., Global prevalence of dementia: a Delphi consensus study. Lancet, 2005. 366(9503): p. 2112-7.
  • Moghul, S. and D. Wilkinson, Use of acetylcholinesterase inhibitors in Alzheimer's disease. Expert Rev Neurother, 2001. 1(1): p. 61-9.
  • Hitesh, N.P., et al., UV-spectrophotometric method development and validation forestimation of Galantamine Hydrobromide in tablet dosage form. Journal of chemical and pharmaceutical research, 2010. 2.
  • Patel, A.V., et al., Determination of galantamine hydrobromide in bulk drug and pharmaceutical dosage form by spectrofluorimetry. J Pharm Bioallied Sci, 2013. 5(4): p. 314-7.
  • Rizzi, A., et al., Enantiomeric resolution of galanthamine and related drugs used in anti-Alzheimer therapy by means of capillary zone electrophoresis employing derivatized cyclodextrin selectors. J Chromatogr B Biomed Sci Appl, 1999. 730(2): p. 167-75.
  • Hsieh, Y.H., et al., Simultaneous determination of galantamine, rivastigmine and NAP 226-90 in plasma by MEKC and its application in Alzheimer's disease. Electrophoresis, 2009. 30(4): p. 644-53.
  • Mol, R., et al., Micellar electrokinetic chromatography-electrospray ionization mass spectrometry for the identification of drug impurities. J Chromatogr B Analyt Technol Biomed Life Sci, 2006. 843(2): p. 283-8.
  • Claessens, H.A., et al., High-performance liquid chromatographic determination of galanthamine, a long-acting anticholinesterase drug, in serum, urine and bile. J Chromatogr, 1983. 275(2): p. 345-53.
  • Tencheva, J., I. Yamboliev, and Z. Zhivkova, Reversed-phase liquid chromatography for the determination of galanthamine and its metabolites in human plasma and urine. J Chromatogr, 1987. 421(2): p. 396-400.
  • Mannens, G.S., et al., The metabolism and excretion of galantamine in rats, dogs, and humans. Drug Metab Dispos, 2002. 30(5): p. 553-63.
  • Monbaliu, J., et al., Pharmacokinetics of galantamine, a cholinesterase inhibitor, in several animal species. Arzneimittelforschung, 2003. 53(7): p. 486-95.
  • Long, Z., et al., Strong cation exchange column allow for symmetrical peak shape and increased sample loading in the separation of basic compounds. J Chromatogr A, 2012. 1256: p. 67-71.
  • Petruczynik, A. and M. Waksmundzka-Hajnos, High performance liquid chromatography of selected alkaloids in ion-exchange systems. J Chromatogr A, 2013. 1311: p. 48-54.
  • Verhaeghe, T., et al., Development and validation of a liquid chromatographic-tandem mass spectrometric method for the determination of galantamine in human heparinised plasma. J Chromatogr B Analyt Technol Biomed Life Sci, 2003. 789(2): p. 337-46.
  • Krupesh, P., et al. Quantitative determination of Galantamine Hydrobromide in pharmaceutical dosage form by RP-High Performance Liquid Chromatography. 2010.
  • Nirogi, R.V., et al., Quantitative determination of galantamine in human plasma by sensitive liquid chromatography-tandem mass spectrometry using loratadine as an internal standard. J Chromatogr Sci, 2007. 45(2): p. 97-103.
  • Ravinder, V., et al., A Validated chiral LC Method for the Enantiomeric Separation of Galantamine. Chromatographia, 2008. 67(3): p. 331-334.
  • European Pharmacopoeia 7ed. Vol. 2. 2010.
  • United States Pharmacopeia, . Vol. 34. 2011.
  • Marques, L.A., et al., Stability-indicating study of the anti-Alzheimer's drug galantamine hydrobromide. J Pharm Biomed Anal, 2011. 55(1): p. 85-92.
  • Halpin, C.M., C. Reilly, and J.J. Walsh, Nature's Anti-Alzheimer's Drug: Isolation and Structure Elucidation of Galantamine from Leucojum aestivum. Journal of Chemical Education, 2010. 87(11): p. 1242-1243.

Alternative Analytical Methods for Quantification of Galantamine in Pharmaceuticals

Yıl 2022, , 58 - 64, 31.08.2022
https://doi.org/10.33713/egetbd.1161168

Öz

Objective: For the quantification of galantamine in bulk and pharmaceutical dosage form, new selective, quick, precise, and accurate spectrophotometric and chromatographic procedures were developed and validated.


Material & Methods: Chromatographic separation was performed on an Agilent Extend C18 (250×4.6 mm, 5 µm) column. Ultrapure water containing 0.1% TFA and acetonitrile containing 0.1% TFA (85/15, v/v) were used as mobile phase at a flow rate of 1.0 mL/min. Eluent detection was performed at a wavelength of 288 nm using a UV detector. On the other hand, galantamine was determined by spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 288 nm.


Result: Lambert−Beer plots for galantamine showed linear relationships in the concentration range of 5-30 μg/mL. Both techniques have been statistically evaluated and validated in order to meet the standards of the International Conference on Harmonisation (ICH) and the results showed that spectrophotometric and liquid chromatographic methods were linear, precise, accurate, rugged and robust with RSD values less than 1.00%, and the recovery percentage was within standard limits (98-102%). Then a statistical comparison of these analytical methods was performed. The results of both methods showed no difference and not statistically significant with respect to each other in the 95% confidence interval (p<0.05).


Conclusion: The developed analytical methods were determined to be accurate, highly effective, reliable, fast, simple, and may be employed successfully for routine analysis of galantamine in the bulk as well as pharmaceutical dosage form. They may even be used for quality control analysis and for sample analysis during cleaning validation.

Kaynakça

  • Ferri, C.P., et al., Global prevalence of dementia: a Delphi consensus study. Lancet, 2005. 366(9503): p. 2112-7.
  • Moghul, S. and D. Wilkinson, Use of acetylcholinesterase inhibitors in Alzheimer's disease. Expert Rev Neurother, 2001. 1(1): p. 61-9.
  • Hitesh, N.P., et al., UV-spectrophotometric method development and validation forestimation of Galantamine Hydrobromide in tablet dosage form. Journal of chemical and pharmaceutical research, 2010. 2.
  • Patel, A.V., et al., Determination of galantamine hydrobromide in bulk drug and pharmaceutical dosage form by spectrofluorimetry. J Pharm Bioallied Sci, 2013. 5(4): p. 314-7.
  • Rizzi, A., et al., Enantiomeric resolution of galanthamine and related drugs used in anti-Alzheimer therapy by means of capillary zone electrophoresis employing derivatized cyclodextrin selectors. J Chromatogr B Biomed Sci Appl, 1999. 730(2): p. 167-75.
  • Hsieh, Y.H., et al., Simultaneous determination of galantamine, rivastigmine and NAP 226-90 in plasma by MEKC and its application in Alzheimer's disease. Electrophoresis, 2009. 30(4): p. 644-53.
  • Mol, R., et al., Micellar electrokinetic chromatography-electrospray ionization mass spectrometry for the identification of drug impurities. J Chromatogr B Analyt Technol Biomed Life Sci, 2006. 843(2): p. 283-8.
  • Claessens, H.A., et al., High-performance liquid chromatographic determination of galanthamine, a long-acting anticholinesterase drug, in serum, urine and bile. J Chromatogr, 1983. 275(2): p. 345-53.
  • Tencheva, J., I. Yamboliev, and Z. Zhivkova, Reversed-phase liquid chromatography for the determination of galanthamine and its metabolites in human plasma and urine. J Chromatogr, 1987. 421(2): p. 396-400.
  • Mannens, G.S., et al., The metabolism and excretion of galantamine in rats, dogs, and humans. Drug Metab Dispos, 2002. 30(5): p. 553-63.
  • Monbaliu, J., et al., Pharmacokinetics of galantamine, a cholinesterase inhibitor, in several animal species. Arzneimittelforschung, 2003. 53(7): p. 486-95.
  • Long, Z., et al., Strong cation exchange column allow for symmetrical peak shape and increased sample loading in the separation of basic compounds. J Chromatogr A, 2012. 1256: p. 67-71.
  • Petruczynik, A. and M. Waksmundzka-Hajnos, High performance liquid chromatography of selected alkaloids in ion-exchange systems. J Chromatogr A, 2013. 1311: p. 48-54.
  • Verhaeghe, T., et al., Development and validation of a liquid chromatographic-tandem mass spectrometric method for the determination of galantamine in human heparinised plasma. J Chromatogr B Analyt Technol Biomed Life Sci, 2003. 789(2): p. 337-46.
  • Krupesh, P., et al. Quantitative determination of Galantamine Hydrobromide in pharmaceutical dosage form by RP-High Performance Liquid Chromatography. 2010.
  • Nirogi, R.V., et al., Quantitative determination of galantamine in human plasma by sensitive liquid chromatography-tandem mass spectrometry using loratadine as an internal standard. J Chromatogr Sci, 2007. 45(2): p. 97-103.
  • Ravinder, V., et al., A Validated chiral LC Method for the Enantiomeric Separation of Galantamine. Chromatographia, 2008. 67(3): p. 331-334.
  • European Pharmacopoeia 7ed. Vol. 2. 2010.
  • United States Pharmacopeia, . Vol. 34. 2011.
  • Marques, L.A., et al., Stability-indicating study of the anti-Alzheimer's drug galantamine hydrobromide. J Pharm Biomed Anal, 2011. 55(1): p. 85-92.
  • Halpin, C.M., C. Reilly, and J.J. Walsh, Nature's Anti-Alzheimer's Drug: Isolation and Structure Elucidation of Galantamine from Leucojum aestivum. Journal of Chemical Education, 2010. 87(11): p. 1242-1243.
Toplam 21 adet kaynakça vardır.

Ayrıntılar

Birincil Dil İngilizce
Konular Klinik Tıp Bilimleri
Bölüm Orijinal Araştırma
Yazarlar

Numan Taşpınar 0000-0002-1417-5907

İbrahim Bulduk 0000-0001-6172-7738

Yayımlanma Tarihi 31 Ağustos 2022
Kabul Tarihi 28 Ağustos 2022
Yayımlandığı Sayı Yıl 2022

Kaynak Göster

EndNote Taşpınar N, Bulduk İ (01 Ağustos 2022) Alternative Analytical Methods for Quantification of Galantamine in Pharmaceuticals. Ege Tıp Bilimleri Dergisi 5 2 58–64.

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