食品中甜蜜素定量方法的改进

Improvement in Quantitative Method of Sodium Cyclamate in Food

建立了气相色谱法测定食品中甜蜜素的方法。固体试样经粉碎、超声提取,液体试样取样后水浴加热除去二氧化碳或酒精,反应后采用Gs BP-1毛细管柱（30 m×0.25 mm×0.25μm）分离,气相色谱测定甜蜜素,产生两个反应产物。经气质联用法确认第一个峰为环己醇亚硝酸酯,第二个峰为环己醇,随放置时间的延长,峰1的面积逐渐减小,峰2的面积逐渐增大,两个峰的面积和始终保持不变,根据两峰面积和定量,甜蜜素质量浓度在0.030~1.0 mg/m L内具有较好的线性关系,其线性回归方程为y=298.81x＋1.835,相关系数（R2）为0.999 9,相对标准偏差〈2%,方法的检测限为0.030 g/kg,样品加标回收率为96.3%~103.5%。该方法具有操作简便、快速、准确度较好等特点,适用于食品中甜蜜素的快速测定。

A gas chromatography method for determination of sodium cyclamate in food was developed. The solid substance was crushed and ultrasonic extracted, while liquid substance was heated to remove carbon dioxide or alcohol after sampling. Two reaction products were generated and separated by capillary column GsBP-1 （30 m×0.25 mm×025 μm） and detemained by GC. The spectrum of the first peak was definitely nitrous acid cyclohexylester, the second one was cyclohexanol by gas chromatography-mass spectrometry （GC-MS）. The area of the first peak gradually reduced as the time prolonged, and the second one increased, but the area of two peaks remained the same. The peaks of the two reaction products were both used for calculation. The method exhibited good linearity in the range from 0.030 to 1.0 mg/mL with the correlation coefficient of 0.999 9, and linear equation was y=298.81x＋ 1.835. The recovery rate of the method was 96.3%~103.5%; the precision （RSD） was less than 2%; the detection limit was 0.030 g/kg. The results showed that this method was simple, rapid and accurate with high recovery. It could be used to quickly determine sodium cyclamate in food.