Tablet dozaj formlarında bulunan tenofovir disoproksil ve emtrisitabinin hidrofilik etkileşimli yüksek performans sıvı kromatografisi yöntemi ile bir arada tayini
Küçük Resim Yok
Tarih
2024
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Trakya Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
"Tablet Dozaj Formlarında Bulunan Tenofovir Disoproksil ve Emtrisitabinin HILIC-HPLC Yöntemi ile Bir Arada Tayini", Trakya Üniversitesi Sağlık Bilimleri Enstitüsü, Farmasötik Nanoteknoloji Anabilim Dalı, Yüksek Lisans, Edirne, 2023. Tenofovir disoproksil fumarat ve emtrisitabin yetişkinlerde insan immün yetmezlik virüsü ve hepatit B virüslerine karşı kullanılmakta olan antiviral etkin maddelerdir. Tedavide sıklıkla birlikte kullanılmakta olan bu ilaçlar hastalara kombine tablet dozaj formunda reçete edilmektedir. Yüksek performanslı sıvı kromatografisi karmaşık numunelerde bulunan analitlerin miktar tayinlerinin sağlanmasında yaygın olarak kullanılan bir tekniktir. Hidrofilik etkileşim kromatografisi polar özellik gösteren küçük moleküllerin analizinde başarı ile uygulanan bir yöntemdir. Yapılan bu çalışmada kombine tablet dozaj formu içerisinde bulunan tenofovir disoproksil fumarat ve emtrisitabin etkin maddelerinin yüksek performanslı sıvı kromatografisi tekniği ile hidrofilik etkileşim kolonu kullanılarak miktar tayini yöntemi geliştirilmiş ve yöntem validasyonu sağlanmıştır. Geliştirilen kromatografik yöntem ticari olarak satılan ürün üzerinde uygulanarak, ürün içeriğinde bulunan tenofovir diproksil fumarat ve emtrisitabinin kromatografik analizi gerçekleştirilmiştir. Analiz yüksek performanslı sıvı kromatografi-diyod sıralı dedektör sistemi kullanılarak gerçekleştirilmiştir. Etkin maddelerin kromatografik ayırımının sağlanması için uygun hareketli faz bileşimi, akış hızı ve analiz sıcaklığı belirlenmiştir. Yöntem validasyonu özgünlük, doğrusallık, gözlenebilme sınırı, tayin sınırı, doğrusal aralık, doğruluk, kesinlik ve sağlamlık çalışmaları ile gerçekleştirilmiştir. Kromatografik analiz hareketli faz olarak asetonitril:amonyum asetat tamponu (100mM) 85:15 (h:h) ve HILIC amid kolon kullanılarak gerçekleştirilmiştir. Ayırım 0,4 ml.dk.- 1 akış hızında, 10 µL enjeksiyon hacminde, 25 ?C sıcaklıkta sağlanmıştır. Dedeksiyon dalga boyları tenofovir diproksil fumarat için 260 nm, emtrisitabin için 284 nm olarak tespit edilmiştir. Alıkonma süreleri tenofovir diproksil fumarat için 4,34 dakika, emtrisitabin için 7,58 dakikadır. Tenofovir diproksil fumarat için gözlenebilme sınırı 0,149 µg.ml-1 , tayin sınırı 0,352 µg.ml-1 ; emtrisitabin için gözlenebilme sınırı 0,108 µg.ml-1 , tayin sınırı 0,327 µg.ml-1 olarak tespit edilmiştir. Geliştirilen yöntem validasyonu kapsamında, etkin maddelerin özgünlük (Rs>1,5), doğrusallık (R2?0,999), doğruluk (% geri kazanım = % 98-102), kesinlik (% BSS<% 2), ve sağlamlık çalışmaları için yasal düzenleme kriterlerini sağladığı tespit edilmiştir. Ticari üründe bulunan tenofovir diproksil fumaratın % 99,17, emtrisitabin ise % 101,58 analiz yüzdeleri ile miktar tayinleri sağlanmıştır. Anahtar kelimeler: HILIC, HPLC, Antiviral, Tenofovir Disoproksil Fumarat, Emtrisitabin, Destekleyen Kurum: Bu çalışma, Trakya Üniversitesi Bilimsel Araştırma Projeleri Birimi tarafından desteklenmiştir. Proje No: 2021/138
Determination of Tenofovir Disoproxil and Emtricitabine in Tablet Dosage Forms by HILIC-HPLC Method", Trakya University Institute of Health Sciences, Department of Pharmaceutical Nanotechnology, Master's Degree, Edirne, 2023. Tenofovir disoproxil fumarate and emtricitabine are antiviral active ingredients used against human immunodeficiency virus and hepatitis B viruses in adults. These drugs, which are often used together in treatment, are prescribed to patients in combined tablet dosage form. High performance liquid chromatography is a widely used technique for the quantification of analytes in complex samples. Hydrophilic interaction chromatography has been successfully applied to analyze small molecules with polar properties. In this study, a method for the quantification of the active substances tenofovir disoproxil fumarate and emtricitabine in the combined tablet dosage form using hydrophilic interaction column with high performance liquid chromatography technique was developed and method validation was provided. The developed chromatographic method was applied on a commercially available product and chromatographic analysis of tenofovir diproxyl fumarate and emtricitabine in the product content was performed. The analysis was performed using a high-performance liquid chromatography-diode array detector system. Suitable mobile phase composition, flow rate and analysis temperature were determined to ensure chromatographic separation of active substances. Method validation was performed with specificity, linearity, limit of observability, limit of detection, linear range, accuracy, precision and robustness studies. Chromatographic analysis was performed using acetonitrile:ammonium acetate buffer (100 mM) 85:15 (h:h) and HILIC amide column as mobile phase. Separation was achieved at a flow rate of 0.4 ml.min.-1 , injection volume of 10 µL, temperature 25 ?C. Detection wavelengths were 260 nm for tenofovir diproxyl fumarate and 284 nm for emtricitabine. The retention times were 4.34 minutes for tenofovir diproxyl fumarate and 7.58 minutes for emtricitabine. The detection limit for tenofovir diproxil fumarate was 0.149 µg.ml-1 and the limit of detection was 0.352 µg.ml-1 ; the detection limit for emtricitabine was 0.108 µg.ml-1 and the limit of detection was 0.327 µg.ml-1 . Within the scope of the developed method validation, it was determined that the active substances met the regulatory criteria for specificity (Rs>1.5), linearity (R2 ?0.999), accuracy (% recovery = 98-102%), precision (% BSS<2%),and robustness studies. Tenofovir diproxil fumarate and emtricitabine in the commercial product were quantified with 99.17% and 101.58% analysis percentages, respectively. Keywords: HILIC, HPLC, Antiviral, Tenofovir Disoproxil Fumarate, Emtricitabine, Supporting Institution: This study was supported by Trakya University Scientific Research Projects Unit. Project No: 2021/138
Determination of Tenofovir Disoproxil and Emtricitabine in Tablet Dosage Forms by HILIC-HPLC Method", Trakya University Institute of Health Sciences, Department of Pharmaceutical Nanotechnology, Master's Degree, Edirne, 2023. Tenofovir disoproxil fumarate and emtricitabine are antiviral active ingredients used against human immunodeficiency virus and hepatitis B viruses in adults. These drugs, which are often used together in treatment, are prescribed to patients in combined tablet dosage form. High performance liquid chromatography is a widely used technique for the quantification of analytes in complex samples. Hydrophilic interaction chromatography has been successfully applied to analyze small molecules with polar properties. In this study, a method for the quantification of the active substances tenofovir disoproxil fumarate and emtricitabine in the combined tablet dosage form using hydrophilic interaction column with high performance liquid chromatography technique was developed and method validation was provided. The developed chromatographic method was applied on a commercially available product and chromatographic analysis of tenofovir diproxyl fumarate and emtricitabine in the product content was performed. The analysis was performed using a high-performance liquid chromatography-diode array detector system. Suitable mobile phase composition, flow rate and analysis temperature were determined to ensure chromatographic separation of active substances. Method validation was performed with specificity, linearity, limit of observability, limit of detection, linear range, accuracy, precision and robustness studies. Chromatographic analysis was performed using acetonitrile:ammonium acetate buffer (100 mM) 85:15 (h:h) and HILIC amide column as mobile phase. Separation was achieved at a flow rate of 0.4 ml.min.-1 , injection volume of 10 µL, temperature 25 ?C. Detection wavelengths were 260 nm for tenofovir diproxyl fumarate and 284 nm for emtricitabine. The retention times were 4.34 minutes for tenofovir diproxyl fumarate and 7.58 minutes for emtricitabine. The detection limit for tenofovir diproxil fumarate was 0.149 µg.ml-1 and the limit of detection was 0.352 µg.ml-1 ; the detection limit for emtricitabine was 0.108 µg.ml-1 and the limit of detection was 0.327 µg.ml-1 . Within the scope of the developed method validation, it was determined that the active substances met the regulatory criteria for specificity (Rs>1.5), linearity (R2 ?0.999), accuracy (% recovery = 98-102%), precision (% BSS<2%),and robustness studies. Tenofovir diproxil fumarate and emtricitabine in the commercial product were quantified with 99.17% and 101.58% analysis percentages, respectively. Keywords: HILIC, HPLC, Antiviral, Tenofovir Disoproxil Fumarate, Emtricitabine, Supporting Institution: This study was supported by Trakya University Scientific Research Projects Unit. Project No: 2021/138
Açıklama
Yüksek Lisans
Anahtar Kelimeler
Eczacılık ve Farmakoloji, Pharmacy and Pharmacology
