Metode sensitif dan tervalidasi untuk penentuan melamin dan asam sianurat dalam susu formula dikembangkan menggunakan kromatografi cair kinerja tinggideteksi diode array (HPLC-PDA) dengan ekstraksi fasa-padat (solid-phase extractor). Kondisi ekstraksi, SPE, dan KCKT diteliti dan dioptimisasi. Linearitas dalam konsentrasi 0,25-5,00 μg/mL memiliki koefisien korelasi 0,9951 untuk asam sianurat standar dan 0,9987 untuk melamin standar. Pada kondisi optimal, batas deteksi (limit of detection/LOD) dan batas kuantifikasi (limit of quantification/LOQ) untuk asam sianurat adalah 0,668 ppm dan 2,227 ppm; dan untuk melamin adalah 0,280 ppm dan 0,934 ppm. Temu balik melamin pada sampel susu yang ditambahkan dengan 24,7-100,2 mg/L diketahui sebesar 96,73- 99,46% dengan SBR (n = 3) 6,458-8,745%. Suatu optimisasi dan metode validasi untuk penentuan melamin dan asam sianurat dalam sampel susu formula didapatkan dan telah diterapkan dengan baik.
A sensitive and validated method for the determination of melamin and cyanuric acid in formula milk is developed using high-performance liquid chromatographydiode array detection (HPLC-DAD) with solid-phase extraction (SPE). The conditions of the extraction, SPE, and HPLC were investigated and optimized. The linearity of satisfactory in the range of 0,25-5,00 μg/mL with a correlation coefficient of 0,9951 for cyanuric acid standard and 0,9987 for melamine. Under the optimal condition, the method limit of detection (LOD) and method limit of quantification (LOQ) for cyanuric acid were 0,668 ppm and 2,227 ppm; and for melamine were 0,280 ppm and 0,934 ppm, respectively. The recovery of melamine for milk samples spiked with 24,7-100,2 mg/L was in the range of 96,73-99,46% with the RSDs (n = 3) of 6,458-8,745%. An optimization and validation method for determination of melamine and cyanuric acid in formula milk samples was achieved and has been applied successfully. |
