Determination of Residual Methanol in Sucralose by Gas Chromatography / 中国药房

ABSTRACT

OBJECTIVE:To establish a method for the determination of residual methanol in sucralose. METHODS:Head-space capillary GC method was adopted. The determination was performed on DB-624 capillary column by temperature program-ming(initial temperature of 35 ℃,maintaining for 5 min,then raising to 200 ℃ at a rate of 50 ℃/min,maintaining for 5 min), the detector was FID. The temperature of the injector was maintaining at 220 ℃ and that of detector at 250 ℃,carrier gas was ni-trogen gas at the flow rate of 2.0 ml/min,the split ratio was 10∶1,headspace temperature was 80 ℃ and equilibrium time was 30 min,and the volume was 1 ml. RESULTS:The linear range of methanol was 98.99-296.96 μg/ml(r=0.999 9);RSDs of preci-sion,stability and reproducibility tests were all no more than 2.16%;the average recoveries were 100.20%(RSD=0.48%,n=9). The limit of detection(LOD)of sucralose was 1.39 μg/ml. In samples from 3 manufacturers,the contents of residual methanol in one manufacturer were 3.12 μg/ml,and the other two were lower than LOD. CONCLUSIONS:This method is simple and fast, and suitable for the determination of residual methanol in sucralose.