Validasi Metode Analisa Penetapan Kadar Amoksisilin dengan Kromatografi Cair Kinerja Tinggi dalam Sediaan Injeksi Kering

Validation of a Method for Determining the Amoxicillin Concentration in Dry Injection Preparations Using High-Performance Liquid Chromatography

Abstract

Amoxicillin is a β-lactam antibiotic commonly used in the treatment of bacterial infections and is available in parenteral dosage forms, including dry powder for injection. The conformity of active ingredient content in parenteral preparations is an important aspect of ensuring drug quality and dose accuracy. Therefore, an accurate and precise analytical method is required to ensure reliable assay results. High-Performance Liquid Chromatography (HPLC) is widely used for the analysis of amoxicillin because of its good separation and quantification capabilities. However, the analytical method must be validated to ensure its suitability for the intended analytical purpose and the characteristics of the dosage-form matrix. This study aimed to validate an HPLC method for the assay of amoxicillin in a 1 g/vial dry powder for injection manufactured by a private pharmaceutical company. The study was conducted experimentally using a Bondapak C18 column (4.6 × 150 mm), a mobile phase consisting of sodium dihydrogen phosphate buffer at pH 4.4 and methanol (93:7), a flow rate of 1.5 mL/min, and a maximum absorption wavelength of 230 nm. The validation parameters included linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. The results showed an r value of 0.9999, a limit of detection (LOD) of 7.733 µg/mL, a limit of quantification (LOQ) of 25.778 µg/mL, a precision of ≤2% RSD, and an accuracy of 98.58–101.61%. The mean amoxicillin content in the samples was 102.87%. The HPLC method met the validation criteria and can be used for the accurate and precise assay of amoxicillin in dry powder for injection.

ABSTRAK

Amoksisilin merupakan antibiotik β-laktam yang sering digunakan dalam pengobatan infeksi bakteri dan tersedia dalam bentuk sediaan parenteral, termasuk injeksi kering. Kesesuaian kadar zat aktif pada sediaan parenteral merupakan aspek penting dalam menjamin mutu dan ketepatan dosis obat. Oleh karena itu, diperlukan metode analisis yang akurat dan presisi untuk memastikan hasil penetapan kadar dapat diandalkan. Kromatografi Cair Kinerja Tinggi (KCKT) banyak digunakan dalam analisis amoksisilin karena memiliki kemampuan pemisahan dan kuantifikasi yang baik. Namun, metode analisis perlu divalidasi untuk memastikan kesesuaiannya terhadap tujuan analisis dan karakteristik matriks sediaan. Penelitian ini bertujuan memvalidasi metode KCKT untuk penetapan kadar amoksisilin dalam sediaan injeksi kering 1 g/vial produksi industri farmasi swasta. Penelitian dilakukan secara eksperimental menggunakan kolom Bondapak C18 (4,6 × 150 mm), fase gerak buffer natrium dihidrogen fosfat pH 4,4 dan metanol (93:7), laju alir 1,5 mL/menit dengan panjang gelombang maksimal 230 nm. Parameter validasi meliputi linearitas, BD, BK, presisi, dan akurasi. Hasil menunjukkan nilai r sebesar 0,9999, BD 7,733 µg/mL, BK 25,778 µg/mL, %RSD presisi ≤2%, dan akurasi 98,58–101,61%. Kadar rata-rata sampel amoksisilin sebesar 102,87%. Metode KCKT memenuhi kriteria validasi dan dapat digunakan untuk penetapan kadar amoksisilin dalam sediaan injeksi kering secara akurat dan presisi.