TEMEL BİLEŞEN REGRESYONU VE KISMİ EN KÜÇÜK KARELER REGRESYONU MODELLERİ KULLANILARAK ATORVASTATİN VE EZETİMİBİN İKİLİ KARIŞIMLARDA EŞZAMANLI TAYİNİ

Yıl 2025, Cilt: 49 Sayı: 3, 827 - 837, 19.09.2025

Zehra Ceren Ertekin , Erdal Dinç

https://doi.org/10.33483/jfpau.1666211

Öz

Amaç: Atorvastatin (AT) ve ezetimibin (EZ) kombinasyonu gibi sabit dozlu formülasyonlardaki etken maddelerin spektral örtüşmeleri, UV-GB spektroskopi temelli analiz yöntemlerinin geliştirilmesini zorlaştırır. Geleneksel kromatografik yöntemler bu tür durumlarda etkili olsa da, maliyet açısından verimli değildir ve gerekli cihazlara erişim kolay olmayabilir. Bu çalışma, sabit dozlu formülasyonlarda AT ve EZ'in eş zamanlı miktar tayini için daha basit ve ekonomik bir spektrofotometri temelli yaklaşım geliştirmeyi amaçlamaktadır.
Gereç ve Yöntem: Bu çalışmada, temel bileşen regresyonu (PCR) ve kısmi en küçük kareler regresyonu (PLS) modelleri, UV-GB spektroskopisi ile birlikte kullanılmıştır. Her iki ilaç için de 4–36 µg/ml çalışma aralığında ikili karışımlardan oluşan bir kalibrasyon seti hazırlanmıştır. PCR ve PLS modelleri üç gizli değişken kullanılarak oluşturulmuştur. Geliştirilen yöntemler, laboratuvarda hazırlanan örnekler kullanılarak doğruluk, kesinlik ve seçicilik açısından değerlendirilmiştir. Yöntemlerin uygulanabilirliği, ticari tablet örnekleri analiz edilerek gösterilmiştir.
Sonuç ve Tartışma: Her iki modelle yüksek geri kazanım oranları (%98–102.3) ve düşük bağıl standart sapma değerleri (<%2.0) elde edilmiş, yöntemlerin doğruluk ve kesinliklerini doğrulamıştır. Yöntemlerin seçiciliği, standart ekleme çalışmaları ile teyit etmiştir. Kapsamlı numune hazırlama gerektirmeden, PCR ve PLS yöntemleri kullanılarak film kaplı tabletlerdeki AT ve EZ'in eş zamanlı miktar tayinleri başarıyla gerçekleştirilmiştir. Geliştirilen yöntemler, geleneksel tekniklere kıyasla basit, ekonomik ve verimli alternatifler sunmuştur.

Anahtar Kelimeler

Atorvastatin , ezetimib , kemometri , PCR , PLS , spektrofotometri

SPECTROPHOTOMETRIC CO-ESTIMATION OF ATORVASTATIN AND EZETIMIBE IN A BINARY MIXTURE USING PRINCIPLE COMPONENT REGRESSION AND PARTIAL LEAST SQUARES REGRESSION MODELS

Öz

Objective: Fixed-dose formulations, such as combination of atorvastatin (AT) and ezetimibe (EZ), present analytical challenges due to overlapping spectral features in UV-Vis spectroscopy. Although traditional chromatographic methods are effective in these cases, they are not cost-efficient, and the required instrumentation is not easily accessible. This study aims to develop a simpler, cost-effective spectrophotometry-based approach for the simultaneous quantification of AT and EZ in fixed-dose formulations.
Material and Method: Principal component regression (PCR) and partial least squares (PLS) regression models were used in combination with UV-Vis spectroscopy. A calibration set of binary mixtures was prepared in the working range of 4–36 µg/ml for both drugs. PCR and PLS models were constructed using three latent variables. The developed methods were evaluated for accuracy, precision, and selectivity using laboratory-prepared samples. The applicability of the methods was demonstrated by analyzing commercial tablet samples.
Result and Discussion: Both models achieved high recovery rates (98–102.3%) and low relative standard deviations (<2.0%), confirming their accuracy and precision. Standard addition studies confirmed the selectivity of the methods. Then, the proposed PCR and PLS methods successfully quantified AT and EZ in commercial film-coated tablets without extensive sample preparation, offering a simple, cost-effective, and efficient alternative to conventional techniques.

Anahtar Kelimeler

Atorvastatin , chemometrics , ezetimibe , PCR , PLS , spectrophotometry

Kaynakça

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