PENGEMBANGAN METODE PENETAPAN KADAR SIKLAMAT BERBASIS KROMATOGRAFI CAIR KINERJA TINGGI GUNA DIIMPLEMENTASIKAN DALAM KAJIAN PAPARAN

Abstract

The aim of this research was to develop a method for determining cycla­mate content in foods based on High Performance Liquid Chromatography for exposure assessment of cyclamate. The extraction procedure is conducted by de­creasing pH sample until less than 2, and mobile phase is executed by applying the ratio of phosphate buffer-methanol as 75:25, 80:20, 85:15. The results of experiments be obtained colom: ODS RP-18, 5 μm, 250 x 4,6 mm ID; mobile phase: phosphate buffer/KH₂PO₄ pH 4,6 and metanol in a ratio of 85:15; flow rate: 1 ml/min; injection volume: 20 μl; and detector: UV-Vis 200 nm. The indication of extraction showed by parameter distribution ratio D ≈ K_D and the extraction efficiency of 83.04–94.92%. The exposure estimated of cyclamate based concentration analysis is about 28.41 mg/kg bw/day (258.27% ADI), where SNI 01-6993-2004 regulates 2.99 mg/kg bw/day (27.21% ADI).

Tujuan penelitian adalah mengembangkan metode penetapan siklamat ber­basis kromatografi cair kinerja tinggi untuk pengukuran konsentrasi siklamat. Prose­dur  ekstraksi menggunakan  modifikasi  pH sampel hingga pH lebih kecil 2, dan fase gerak diterapkan perlakuan rasio bufer fosfat–metanol 75 : 25, 80 : 20, dan 85 : 15. Hasil eksperimen diperoleh kolom: ODS RP-18, 5 μm, 250 x 4,6 mm ID; fase gerak: bufer fosfat/KH₂PO₄ pH 4,6 dan metanol rasio 85 : 15; laju aliran: 1 ml/menit; volume injeksi: 20 μl; dan detektor: UV-Vis 200 nm. Indikasi keberhasilan ekstraksi ditunjukkan dengan parameter rasio distribusi D ≈ K_D dan efisiensi ekstraksi 83,04–94,92%. Estimasi paparan berdasar konsentrasi analisis langsung sebesar 28,41 mg/kg bb/hari (258,27% ADI), sedang estimasi paparan berbasis SNI 01-6993-2004 sebesar 2,99 mg/kg bb/hari (27,21% ADI).