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İnsan İdrarında Valasiklovirin Tayini için RPLC Yöntemin Geliştirilmesi ve Validasyonu

Year 2023, Volume: 14 Issue: 2, 282 - 291, 15.08.2023

Yaşar Doğan Daldal

https://doi.org/10.22312/sdusbed.1311241

Abstract

Sunulan çalışmada, herpes ve megalovirüslerin sebep olduğu enfeksiyonların tedavisinde tercihli olarak kullanılan ilaçlardan valasiklovirin katkılandırılmış idrarda ters faz sıvı kromatografik yöntemle tayini için yöntem geliştirilmiştir. Yöntem geliştirmede, valasiklovirin sistematik olarak pH-kapasite faktörü ilişkisini değerlendirilip, mobil faz optimizasyonu gerçekleştirilmiştir. İnceleme sonunda, optimum ayırma koşulu %4 asetonitril-su (h/h), pH 5,0 ve 37oC kolon sıcaklığı olarak belirlenmiştir. Sonrasında, belirlenen optimum koşulun Uluslararası Harmonizasyon Topluluğu (ICH) yönergelerine göre validasyonu gerçekleştirilmiştir. Geliştirilen yöntem 2-12 μg/mL derişim aralığında muhteşem doğrusallık göstermiştir ve idrar ortamında gerçekleştirilen geri kazanma sonuçları (%) valasiklovirin iki farklı derişimi için 100,147±0,800 ve 100,208±0,604 olarak bulunmuştur. Ayrıca, geliştirilen yönteme sağlamlık testleri de uygulanmıştır ve elde edilen sonuçlar t-testiyle değerlendirilmiştir. Elde edilen validasyon ve sağlamlık testleri sonucunda, geliştirilen yöntemin hassas, tekrar edilebilir, doğru, kesin ve sağlam olduğu bulunmuştur. Bundan dolayı, geliştirilen yöntemin rutin analizler için uygun olduğu belirlenmiştir.

Keywords

Antiherpes valasiklovir metot geliştirme pKa RPLC

Supporting Institution

Kahramanmaraş İstiklal Üniversitesi Bilimsel Araştırma Projeleri Koordinasyon Birimi (BAP)

Project Number

2021/3-1 BAP

References

  • [1] Kayaalp, O. 2000. Rasyonel Tedavi Yönünden Tıbbi Farmakoloji. 9th, edition. Hacettepe-Taş Kitapçılık Ltd. Şti. Ankara, 880s.
  • [2] Hilal-Dandan, R., Laurence, L. B. 2017. Goodman & Gillman Tedavinin Farmakolojik Temeli. 2nd, edition. Güneş Tıp Kitapevleri, Ankara, 1205s.
  • [3] Katzung, B. G. 2011. Basic & Clinical Pharmacology. 12th, edition. The McGraw-Hill Companies, San Francisco, 1245s.
  • [4] Dar, B. P. W., Öksüz, Z., Algül, Ö. 2019. Antiviral İlaçlardaki Gelişmeler ve Değerlendirilmesi. Lokman Hekim Dergisi, 9(2),160-170.
  • [5] Kazakevich, Y., Lobrutto, Y. 2007. HPLC for Pharmaceutical Scientists. 1st, edition. Wiley-Interscience, Canada, 1135s.
  • [6] Uysal, R., Daldal, Y. D., Üstün, Z., Demiralay, E. Ç. 2017. Optimization of RPLC Method for Separation of Some Acetylcholinesterase Inhibitors by Using Central Composite Design. Eurasian Journal of Analytical Chemistry, 2(1), 23-43.
  • [7] Kuzucanli, E., Demiralay, E. Ç., Daldal, Y. D., Üstün, Z., Konçe, İ., Alsancak,G. 2022. Development and Validation of RPLC Method for The Simultaneous Analysis of ACE İnhibitors in Tablet Formulations. Turkish Journal of Chemistry, 4(2),103–110.
  • [8] Gündoğan, B., Demiralay, E. Ç., Daldal, Y. D., Üstün, Z. 2017. Determination of Optimum Separation Condition for Some Carbapenem Antibiotics Using RPLC with the Aid of Central Composite Design and Desirability Function. Current Pharmaceutical Analysis, 13, 100-109.
  • [9] Demiralay, E. Ç. 2012. An Experimental Design Approach to Optimization of the Liquid Chromatographic Separation Conditions for the Determination of Metformin and Glibenclamide in Pharmaceutical Formulation. Acta Chimica Slovenica, 59(2), 307-314.
  • [10] Bosch, M. E., Sánchez, A. J. R., Rojas, F. S., Ojeda C. B. 2009. Ganciclovir: A Review of its Analytical Determination. Asian Journal of Pharmaceutical Sciences, 4(4),254-264.
  • [11] Sheetal Ramya Lahari, N. A. 2013. Method Development and Validation of Valacyclovir in Bulk & Tablet Dosage Form by RPHPLC Method. IOSR journal of pharmacy, 5(1), 56-75.
  • [12] Ganesh, M., Bhagiyalakshmi, M., Hemalatha, P., Rao, C. V. N., Jang, H. T., Rajasekar, K. 2011. RP-HPLC Estimation of Valacyclovir HCl in Tablet Formulation. Asian Journal of Chemistry, 23(3), 1317-1320.
  • [13] Rasool, S. K., Naik, D. V., Babu, D. P., Nallurı, B. N. 2012. RP-HPLC Method for The Estimation of Valacyclovir in Bulk and Pharmaceutical Formulations. International Journal of Pharmacy and Pharmaceutical Sciences, 4(1), 214-218.
  • [14] Patil, G. D., Yeole, P. G., Puranik, M., Wadher, S. J. 2009. A Validated Specific Reverse Phase Liquid Chromatographic Method for the Determination of Valacyclovir in the Presence of its Degradation Products in Bulk Drug and in Tablet Dosage Form. International Journal of ChemTech Research, 1(1), 16-26.
  • [15] Prasad Reddy, D.V., Gurupadayya, B.M., Manohara, Y.N., Vıjaya Bhaskar, V. 2007. Spectrophotometric Determination of Valacyclovir Hydrochloride in Bulk and Pharmaceutical Formulations. Asian Journal of Chemistry, 19(4), 2797-2800.
  • [16] Palacios, M.L., Demasi, G., Pizzorno, M.T., Segall, A.I. 2005. Validation of an HPLC Method for the Determination of Valacyclovir in Pharmaceutical Dosage. Journal of Liquid Chromatography & Related Technologies, 28(5), 751-762.
  • [17] Morgan, E.M., Lotfy, H.M., Fayez, Y.M., Abdelkawy, M. 2022. Comparative Study of the Selectivity Power of Colorimetric Method Over Chromatographic Methods for the Analysis of Valaciclovir Hydrochloride. Journal of AOAC INTERNATIONAL, 105(3), 717–726.
  • [18] Caglar, S. 2014. Determination of Valacyclovir Hydrochloride in Tablets and Spiked Plasma Samples by Spectrofluorimetry. Journal of Analytical Chemistry, 69, 362–366.
  • [19] Savaşer, A., Özkan, C.K., Özkan, Y., Uslu, B., Özkan, S.A. 2003. Development and Validation of an RP‐HPLC Method for the Determination of Valacyclovir in Tablets and Human Serum and Its Application to Drug Dissolution Studies. Journal of Liquid Chromatography & Related Technologies, 26(11), 1755-1767.
  • [20] Darville, J. M., Lovering, A. M., MacGowan, A.P. 2007. Development, Evaluation and Application of An Isocratic High-Performance Liquid Chromatography (HPLC) Assay for The Simultaneous Determination of Aciclovir and its Metabolite 9-Carboxymethoxymethylguanine in Human Serum and Cerebrospinal Fluid. International Journal of Antimicrobial Agents, 30, 30–33.
  • [21] Kasiari, M., Gikas, E., Georgakakou, S., Kazanis, M., Panderi, I. 2007. Selective and Rapid Liquid Chromatography/Negative-İon Electrospray İonization Mass Spectrometry Method for The Quantification of Valacyclovir and its Metabolite in Human Plasma. Journal of Chromatography B, 864, 78–86.
  • [22] Çubuk Demiralay, E., Koç, D., Daldal, Y.D., Alsancak, G., Ozkan, S.A. 2014. Determination of chromatographic dissociation constants of some carbapenem group antibiotics and quantification of these compounds in human urine. Biomedical Chromatography, 28(5), 660-666
  • [23] Rajeswari, K. R., Nageswararao, P., Sankar, G. G., Rao, A. L., Raju, D. B., Rao, J. L. N. S. 2006. Estimation of Valacyclovir in Tablets and Human Serum by RP-HPLC Method. Asian Journal of Chemistry, 18(4), 2515-2518. [24] Chemicalize program. http://www.chemicalize.org (Erişim Tarihi: 02.06.2023).
  • [25] SwissADME program. http://www.swissadme.ch (Erişim Tarihi: 04.08.2023).
  • [26] Volná, T., Motyka, K., Hlaváč, J. 2017. RP-HPLC Determination of Dissociation Constant Using Solely Aqueous Mobile Phase. Journal of Pharmaceutical and Biomedical Analysis, 134, 143–148.
  • [27] ICH Validation of Analytical Procedures, Text and methodology Q2 (R1), International Conference on Harmonization, 2005.

Development and Validation of the RPLC Method for the Determination of Valaciclovir in Human Urine

Year 2023, Volume: 14 Issue: 2, 282 - 291, 15.08.2023

Yaşar Doğan Daldal

https://doi.org/10.22312/sdusbed.1311241

Abstract

In the present study, a method has been developed for the determination of valaciclovir, one of the preferred drugs for the treatment of infections caused by herpes and megaloviruses, in spiked urine by reversed-phase liquid chromatographic method. In developing the method, the pH-capacity factor relationship of valaciclovir was systematically evaluated and mobile phase optimization was performed. At the end of the examination, the optimum separation condition was determined as 4% acetonitrile-water (v/v), pH 5.0, and 37oC column temperature. Subsequently, the determined optimum condition was validated according to the guidelines of the International Conference on Harmonization (ICH). The developed method showed excellent linearity in the concentration range of 2-12 μg/mL, and the recovery results (%) performed in urine were found to be 100.147±0.800 and 100.208±0.604 for two different concentrations of valaciclovir. In addition, robustness tests were also performed for the developed method and the results were evaluated using the t-test. The results of the validation and robustness tests showed that the developed method is sensitive, reproducible, accurate, precise and robust. Therefore, the developed method was found to be suitable for routine analysis.

Keywords

Antiherpes Valaciclovir method development pKa RPLC

Project Number

2021/3-1 BAP

References

  • [1] Kayaalp, O. 2000. Rasyonel Tedavi Yönünden Tıbbi Farmakoloji. 9th, edition. Hacettepe-Taş Kitapçılık Ltd. Şti. Ankara, 880s.
  • [2] Hilal-Dandan, R., Laurence, L. B. 2017. Goodman & Gillman Tedavinin Farmakolojik Temeli. 2nd, edition. Güneş Tıp Kitapevleri, Ankara, 1205s.
  • [3] Katzung, B. G. 2011. Basic & Clinical Pharmacology. 12th, edition. The McGraw-Hill Companies, San Francisco, 1245s.
  • [4] Dar, B. P. W., Öksüz, Z., Algül, Ö. 2019. Antiviral İlaçlardaki Gelişmeler ve Değerlendirilmesi. Lokman Hekim Dergisi, 9(2),160-170.
  • [5] Kazakevich, Y., Lobrutto, Y. 2007. HPLC for Pharmaceutical Scientists. 1st, edition. Wiley-Interscience, Canada, 1135s.
  • [6] Uysal, R., Daldal, Y. D., Üstün, Z., Demiralay, E. Ç. 2017. Optimization of RPLC Method for Separation of Some Acetylcholinesterase Inhibitors by Using Central Composite Design. Eurasian Journal of Analytical Chemistry, 2(1), 23-43.
  • [7] Kuzucanli, E., Demiralay, E. Ç., Daldal, Y. D., Üstün, Z., Konçe, İ., Alsancak,G. 2022. Development and Validation of RPLC Method for The Simultaneous Analysis of ACE İnhibitors in Tablet Formulations. Turkish Journal of Chemistry, 4(2),103–110.
  • [8] Gündoğan, B., Demiralay, E. Ç., Daldal, Y. D., Üstün, Z. 2017. Determination of Optimum Separation Condition for Some Carbapenem Antibiotics Using RPLC with the Aid of Central Composite Design and Desirability Function. Current Pharmaceutical Analysis, 13, 100-109.
  • [9] Demiralay, E. Ç. 2012. An Experimental Design Approach to Optimization of the Liquid Chromatographic Separation Conditions for the Determination of Metformin and Glibenclamide in Pharmaceutical Formulation. Acta Chimica Slovenica, 59(2), 307-314.
  • [10] Bosch, M. E., Sánchez, A. J. R., Rojas, F. S., Ojeda C. B. 2009. Ganciclovir: A Review of its Analytical Determination. Asian Journal of Pharmaceutical Sciences, 4(4),254-264.
  • [11] Sheetal Ramya Lahari, N. A. 2013. Method Development and Validation of Valacyclovir in Bulk & Tablet Dosage Form by RPHPLC Method. IOSR journal of pharmacy, 5(1), 56-75.
  • [12] Ganesh, M., Bhagiyalakshmi, M., Hemalatha, P., Rao, C. V. N., Jang, H. T., Rajasekar, K. 2011. RP-HPLC Estimation of Valacyclovir HCl in Tablet Formulation. Asian Journal of Chemistry, 23(3), 1317-1320.
  • [13] Rasool, S. K., Naik, D. V., Babu, D. P., Nallurı, B. N. 2012. RP-HPLC Method for The Estimation of Valacyclovir in Bulk and Pharmaceutical Formulations. International Journal of Pharmacy and Pharmaceutical Sciences, 4(1), 214-218.
  • [14] Patil, G. D., Yeole, P. G., Puranik, M., Wadher, S. J. 2009. A Validated Specific Reverse Phase Liquid Chromatographic Method for the Determination of Valacyclovir in the Presence of its Degradation Products in Bulk Drug and in Tablet Dosage Form. International Journal of ChemTech Research, 1(1), 16-26.
  • [15] Prasad Reddy, D.V., Gurupadayya, B.M., Manohara, Y.N., Vıjaya Bhaskar, V. 2007. Spectrophotometric Determination of Valacyclovir Hydrochloride in Bulk and Pharmaceutical Formulations. Asian Journal of Chemistry, 19(4), 2797-2800.
  • [16] Palacios, M.L., Demasi, G., Pizzorno, M.T., Segall, A.I. 2005. Validation of an HPLC Method for the Determination of Valacyclovir in Pharmaceutical Dosage. Journal of Liquid Chromatography & Related Technologies, 28(5), 751-762.
  • [17] Morgan, E.M., Lotfy, H.M., Fayez, Y.M., Abdelkawy, M. 2022. Comparative Study of the Selectivity Power of Colorimetric Method Over Chromatographic Methods for the Analysis of Valaciclovir Hydrochloride. Journal of AOAC INTERNATIONAL, 105(3), 717–726.
  • [18] Caglar, S. 2014. Determination of Valacyclovir Hydrochloride in Tablets and Spiked Plasma Samples by Spectrofluorimetry. Journal of Analytical Chemistry, 69, 362–366.
  • [19] Savaşer, A., Özkan, C.K., Özkan, Y., Uslu, B., Özkan, S.A. 2003. Development and Validation of an RP‐HPLC Method for the Determination of Valacyclovir in Tablets and Human Serum and Its Application to Drug Dissolution Studies. Journal of Liquid Chromatography & Related Technologies, 26(11), 1755-1767.
  • [20] Darville, J. M., Lovering, A. M., MacGowan, A.P. 2007. Development, Evaluation and Application of An Isocratic High-Performance Liquid Chromatography (HPLC) Assay for The Simultaneous Determination of Aciclovir and its Metabolite 9-Carboxymethoxymethylguanine in Human Serum and Cerebrospinal Fluid. International Journal of Antimicrobial Agents, 30, 30–33.
  • [21] Kasiari, M., Gikas, E., Georgakakou, S., Kazanis, M., Panderi, I. 2007. Selective and Rapid Liquid Chromatography/Negative-İon Electrospray İonization Mass Spectrometry Method for The Quantification of Valacyclovir and its Metabolite in Human Plasma. Journal of Chromatography B, 864, 78–86.
  • [22] Çubuk Demiralay, E., Koç, D., Daldal, Y.D., Alsancak, G., Ozkan, S.A. 2014. Determination of chromatographic dissociation constants of some carbapenem group antibiotics and quantification of these compounds in human urine. Biomedical Chromatography, 28(5), 660-666
  • [23] Rajeswari, K. R., Nageswararao, P., Sankar, G. G., Rao, A. L., Raju, D. B., Rao, J. L. N. S. 2006. Estimation of Valacyclovir in Tablets and Human Serum by RP-HPLC Method. Asian Journal of Chemistry, 18(4), 2515-2518. [24] Chemicalize program. http://www.chemicalize.org (Erişim Tarihi: 02.06.2023).
  • [25] SwissADME program. http://www.swissadme.ch (Erişim Tarihi: 04.08.2023).
  • [26] Volná, T., Motyka, K., Hlaváč, J. 2017. RP-HPLC Determination of Dissociation Constant Using Solely Aqueous Mobile Phase. Journal of Pharmaceutical and Biomedical Analysis, 134, 143–148.
  • [27] ICH Validation of Analytical Procedures, Text and methodology Q2 (R1), International Conference on Harmonization, 2005.
There are 26 citations in total.

Details

Primary Language Turkish
Subjects Analytical Chemistry (Other)
Journal Section Araştırma Articlesi
Authors

Yaşar Doğan Daldal 0000-0003-1211-2686

Project Number 2021/3-1 BAP
Publication Date August 15, 2023
Submission Date June 7, 2023
Published in Issue Year 2023 Volume: 14 Issue: 2

Cite

Vancouver Daldal YD. İnsan İdrarında Valasiklovirin Tayini için RPLC Yöntemin Geliştirilmesi ve Validasyonu. Süleyman Demirel Üniversitesi Sağlık Bilimleri Dergisi. 2023;14(2):282-91.
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