气相色谱法测定秋梨膏中的环己基氨基磺酸钠

Determination of Sodium Cyclamate in Autumn Pear Grease by Gas Chromatography

建立了气相色谱法测定秋梨膏中环己基氨基磺酸钠含量的分析方法。对国标GB/T 5009.97-2003《食品中环己基氨基磺酸钠的测定》中的气相色谱法进行优化和改进,针对秋梨膏粘稠、含糖量高的特性,对样品稀释后在酸性、低温环境下与亚硝酸钠发生酯化反应,经毛细管色谱柱分离,由氢火焰离子化检测器测定。方法的检出限为2mg/kg,定量限为7mg/kg。在加标水平为2mg/kg及0.10、0.50和1.00mg/g时的平均添加回收率为90.0%-97.5%,相对标准偏差3.31%-9.05%。衍生物的峰面积与样品浓度在0.05-1.00g/L范围内呈良好的线性关系,相关系数R2=0.9996。该方法操作简便快速,灵敏度高,测定结果准确、可靠,适合秋梨膏中环己基氨基磺酸钠含量的测定。

A method for the determination of sodium cyclamate in autumn pear grease by gas chromatography was developed, which gives optimizations and improvements compared with the gas chromatography method described in GB/T 5009.97-2003-Determination of sodium cyclamate in foods. In light of its characteristics of high-viscosity and high sugar content, we dilute the samples of autumn pear grease first, and then derive them with nitrite sodium under acid and low temperature environment. The cyclohexyl nitrite was separated by capillary chromatographic column and analyzed by flame ionizator detector. The limit of detection is 2mg/kg and the limit of quantitation is 7mg/kg. At 2mg/kg and 0.10, 0.50, 1.00mg/g fortification levels, the average recoveries range from 90.0% to 97.5% with the relative standard deviations from 3.31% to 9.05%. The method shows good linearity over the range assayed 0.05 to 1.00g/L （R2=0.9996）. The method is suitable for determination of sodium cyclamate in autumn pear grease, owing to its advantages of rapidity, sensitivity and accuracy.