Quality by design approach for development and validation of a RP-HPLC method for simultaneous estimation of xipamide and valsartan in human plasma

Abstract

A new rapid, simple, and sensitive RP-HPLC method was carried out through applying Quality by Design approach for determination of xipamide and valsartan in Human plasma. Fractional factorial design was used for screening of four independent factors: pH, flow rate, detection wavelength, and % of MeOH. Analysis of variance (ANOVA) confirmed that flow rate and % of MeOH were only significant. Chromatographic conditions optimization was carried out through using central composite design. Method analysis was performed using BDS Hypersil C8 column (250 × 4.6 mm, 5 μm) and an isocratic mobile phase of MeOH and 0.05 M KH2PO4 buffer pH 3 (64.5:35.5, v/v) at 1.2 mL/min flow rate with UV detection at 240 nm and 10 μL injection volume. According to FDA guidelines, the method was then validated for the determination of the two drugs clinically in human plasma in respect of future pharmacokinetic and bioequivalence simulation studies. The standard curve was linear in the concentration range of 5–100 µg/mL for both drugs, with a determination coefficient (R2) of 0.999. Also, the average recoveries lied within the range from 99.89 to 100.03%. The proposed method showed good predictability and robustness.

Analisis dan Validasi Obat Metformin Dalam Plasma Manusia Menggunakan Metode HPLC

“…Pada dasarnya RP-HPLC merupakan metode pengembangan dari HPLC, terdapat perbedaan pada kedua metode tersebut seperti fase gerak yang digunakan pada RP-HPLC lebih polar daripada fase diam. Terdapat perbedaan yang signifikan terhadap metode HPLC dengan RP-HPLC (Tabel 2) seperti pada penelitian Magdy et al, 2023 yang menggunakan metode HPLC dan Shakoor A et al, 2018 untuk metode RP-HPLC dalam analisis metformin pada plasma darah.…”