毛细管柱气相色谱法测定食品中甜蜜素
Determination of Sodium Cyclamate in Food by GC with Capillary Column
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摘要: 应用毛细管柱气相色谱法测定了食品中甜蜜素。选择弱极性的DB-5型毛细管色谱柱(0.53 mm×30 m,1.0 μm)作为分离柱,采用氢火焰离子化检测器。对固体样品的处理方法改用粉碎机打碎,并按样品的类别分别用水或经石油醚提取去脂后,再用水超声提取,离心分离并过滤后取其滤液供色谱分析。甜蜜素的质量浓度在0.01~1.0 g·L-1范围内与峰面积呈线性相关,检出限(3S/N)为1 ng。在3个浓度水平进行加标回收试验,回收率在90.9%~99.5%之间,测定值的相对标准偏差(n=5)在2.9%~6.8%之间。按此法测定了30个食品样品中甜蜜素的含量,所得测定值与欧盟标准方法(EN 12857)测定值相符。Abstract: GC with capillary column was applied to the determination of sodium cyclamate in food. Weakly polar DB-5 capillary chromatographic column (0.53 mm×30 m, 1.0 μm) was chosen as the separation column, and hydrogen FID was adopted for determination. Treatment of solid sample was modified by crushing with a crusher, extracted ultrasonically with water or with petroleum ether to remove fats and then with water, centrifuging, filtering and the filtrate was use for GC analysis. Linear relationship between values of peak area and mass concentration of sodium cyclamate was kept in the range of 0.01-1.0 g·L-1 with detection limit (3S/N) of 1 ng. Tests for recovery were made at 3 concentration levels of sodium cyclamate standard, giving values of recovery and RSD′s (n=5) in the ranges of 90.0%-99.5% and 2.9%-6.8% respectively. The proposed method was used in the analysis of 30 food samples, giving results of sodium cyclamate contents in consistency with values obtained by the method of EN standard of E12857.