Validasi Metode Penetapan Kadar Vitamin D3 dalam Sediaan Kapsul Lunak menggunakan Metode Kromatografi Cair Kinerja Tinggi

Abstract

Vitamin D3 penting bagi kesehatan sehingga diperlukan metode analisis tervalidasi untuk penetapan kadarnya dalam sediaan farmasi. Penelitian ini bertujan untuk memvalidasi metode kromatografi cair kinerja tinggi (KCKT) dalam penetapan kadar vitamin D3 pada sediaan kapsul lunak. Validasi dilakukan berdasarkan parameter spesifisitas, linearitas, batas deteksi (BD), batas kuantitasi (BK), akurasi, presisi, ketahanan dan ketangguhan sesuai persyaratan United States Pharmacopeia (USP). Hasil penelitian menunjukkan metode bersifat spesifik dengan waktu retensi larutan uji sesuai larutan baku (±3%) dan tanpa gangguan dari blangko maupun plasebo. Nilai linearitas diperoleh dengan koefisien korelasi (r) > 0,99, BD 0,13 ppm, BK 0,8 ppm, akurasi memberikan % recovery pada rentang 90–107%, serta presisi %SBR <2%. Ketahanan menunjukkan kestabilan pada variasi laju alir, suhu kolom, dan pelarut, namun berbeda pada kestabilan larutan. Ketangguhan menunjukkan tidak terdapat perbedaan signifikan antar analis. Dengan demikian, metode KCKT ini memenuhi kriteria validasi USP dan dapat digunakan sebagai metode analisis rutin di PT Nova Chemie Utama.

Vitamin D3 was important for health, so a validated analytical method is needed to determine its content in pharmaceutical preparations. This study aims to validate the high performance liquid chromatography (HPLC) method for determining vitamin D3 levels in soft capsules. Validation was performed based on the parameters of specificity, linearity, limit of detection (LoD), limit of quantitation (LoQ), accuracy, precision, robustness, and ruggedness in accordance with the requirements of the United States Pharmacopeia (USP). The results showed that the method was specific, with the retention time of the test solution corresponding to that of the standard solution (±3%) and without interference from the blank or placebo. Linearity values were obtained with a correlation coefficient (r) >0.99, BD 0.13 ppm, BK 0.8 ppm, accuracy providing % recovery in the range of 90–107%, and precision %SBR <2%. Robustness was maintained under variations in flow rate, column temperature, and solvent, although solution stability showed differences. Ruggedness showed no significant differences between analysts. Therefore, this HPLC method meets USP validation criteria and can be used as a routine analysis method at PT Nova Chemie Utama