High-Performance Liquid Chromatography Method Validation for the Determination of Cyproheptadine Hydrochloride in Tablets / Validasi Metode High Performance Liquid Chromatography Untuk Penetapan Kadar Siproheptadin Hidroklorida Pada Tablet.

Cyproheptadine hydrochloride is an antihistamine drug widely available in tablet dosage forms; therefore, a validated analytical method is required to ensure product quality. This study aimed to develop and validate a Reversed-Phase High Performance Liquid Chromatography (RP-HPLC) method for the determination of cyproheptadine hydrochloride 4 mg in tablets according to ICH Q2(R2) and USP 2024 guidelines. The analysis was performed using an XBridge C18 column (2.1 mm × 50 mm; 3.5 µm) with an isocratic mobile phase of acetonitrile:0.1% acetic acid (60:40), a flow rate of 1.0 mL/min, an injection volume of 10 µL, and PDA detection at 285 nm. Validation parameters included specificity, linearity, accuracy, precision, robustness, LOD and LOQ. The method showed excellent linearity with R² of 0.997, recovery of 100.26%, precision with % RSD of 1.42%, LOD 0.0022% and LOQ of 0.0066%. Specificity testing showed no interfering peaks, while robustness was confirmed for a ±5% change in mobile phase composition (%RSD 1.26% for retention time and 1.97% for peak area) but not for a ±5% change in flow rate, where retention time gave %RSD of 2.14%. The procedure is fit for routine quality control assay of cyproheptadine hydrochloride tablets, with the stated limitation on flow-rate robustness.

Siproheptadin hidroklorida merupakan obat antihistamin yang tersedia luas dalam bentuk tablet, sehingga diperlukan metode analisis tervalidasi untuk menjamin mutu produk. Penelitian ini bertujuan mengembangkan dan memvalidasi metode Reversed-Phase High Performance Liquid Chromatography (RP-HPLC) untuk penetapan kadar siproheptadin hidroklorida 4 mg dalam tablet berdasarkan pedoman ICH Q2(R2) dan USP 2024. Analisis dilakukan menggunakan kolom XBridge C18 (2,1 mm × 50 mm; 3,5 µm) dengan fase gerak asetonitril:asam asetat 0,1% (60:40) secara isokratik, laju alir 1,0 mL/menit, volume injeksi 10 µL, dan deteksi PDA 285 nm. Validasi meliputi spesifisitas, linearitas, akurasi, presisi, robustness, LOD dan LOQ. Metode menunjukkan linearitas yang baik dengan nilai R² 0,997, recovery 100,26%, presisi (% RSD) 1,42%, LOD 0,0022% dan LOQ 0,0066%. Uji spesifisitas menunjukkan tidak adanya puncak pengganggu, dan robustness terpenuhi terhadap perubahan komposisi fase gerak ±5% (% RSD 1,26% untuk waktu retensi dan 1,97% untuk luas area), tetapi tidak terpenuhi terhadap perubahan laju alir ±5% dengan % RSD waktu retensi 2,14%. Prosedur ini layak digunakan untuk analisis rutin pengawasan mutu tablet siproheptadin hidroklorida dengan keterbatasan pada robustness laju alir.