DEVELOPMENT AND VALIDATION OF GREEN RP-HPLC AND SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF ALPELISIB IN BULK AND PHARMACEUTICAL DOSAGE FORMS

Öz

Objective: This study aims to develop and validate green analytical methods, specifically UV spectrophotometry, first-order derivative spectrophotometry, and reverse-phase HPLC (RP-HPLC), for determining Alpelisib (ALP) in bulk and pharmaceutical formulations. By comparing the methods using GAPI and AGREE metrics, the study evaluates their environmental friendliness, precision, and applicability. Material and Method: The UV spectrophotometric and RP-HPLC analyses were conducted using Shimadzu UV 1800 and Agilent 1100 HPLC systems, respectively. The mobile phase for HPLC comprised 0.1% trifluoroacetic acid in water, acetonitrile, and methanol (50:25:25 v/v/v). ALP tablets were prepared and analyzed after dissolution in methanol/water (50:50 v/v) and filtration. Validation was conducted according to ICH guidelines. Result and Discussion: The developed methods showed high precision, robustness, and sensitivity. UV and HPLC methods were effective in determining ALP in both bulk drug and tablet formulations, with detection limits of 0.078 μg/ml for direct UV spectrophotometry and 14 μg/ml for RP-HPLC. Greenness evaluation highlighted the methods' environmental compatibility, making them suitable for sustainable pharmaceutical analysis.

Anahtar Kelimeler

• Alpelisib
• anticancer drug
• greenness evaluation
• RP-HPLC
• spectrophotometric
• validation

FARMASÖTİK DOZAJ FORMLARINDA ALPELİSİB MİKTAR TAYİNİ İÇİN VALİDE EDİLMİŞ YÜKSEK PERFORMANSLI SIVI KROMATOGRAFİK VE SPEKTROFOTOMETRİK YÖNTEM GELİŞTİRİLMESİ

Öz

Amaç: Bu çalışma, Alpelisib’in (ALP) yığın ve farmasötik formlarda tayini için çevreci UV spektrofotometri, birinci derece türev spektrofotometri ve ters faz HPLC (RP-HPLC) yöntemlerini geliştirmeyi ve doğrulamayı amaçlanmıştır. Çalışma yöntemlerin çevre dostu olduğunu, doğruluklarını ve uygulanabilirliklerini değerlendirmek için GAPI ve AGREE metrikleri ile karşılaştırılmıştır. Gereç ve Yöntem: UV spektrofotometrik ve RP-HPLC analizleri sırasıyla Shimadzu UV 1800 ve Agilent 1100 HPLC sistemleri ile gerçekleştirilmiştir. HPLC için mobil faz, %0.1 triflorasetik asit suda, asetonitril ve metanolün (50:25:25 h/h/h) karışımından oluşmaktadır. ALP tabletleri, metanol/su (50:50 h/h) içinde çözülüp filtrelendikten sonra hazırlanmış ve analiz edilmiştir. Doğrulama, ICH kılavuzlarına göre yapılmıştır. Sonuç ve Tartışma: Geliştirilen yöntemler yüksek hassasiyet, dayanıklılık ve duyarlılık göstermiştir. UV ve HPLC yöntemleri kullanılarak ilaç formülasyonlarında ALP’nin tayini yapılmış ve doğrudan UV spektrofotometri için 0.078 μg/ml, RP-HPLC için ise 14 μg/ml olarak tespit limitlerine ulaşılmıştır. Çevreci değerlendirme, yöntemlerin sürdürülebilir farmasötik analiz için çevre dostu uyumluluğunu vurgulamaktadır.

Anahtar Kelimeler

• Alpelisib
• antikanser ilaç
• çevreci değerlendirme
• doğrulama
• RP-HPLC
• spektrofotometrik

Kaynakça

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