气相色谱法测定馒头中甜蜜素的干扰消除

Eliminating interference of determining of sodium cyclamate in steamed bread by gas chromatography

目的比较不同条件下气相色谱仪测定馒头中甜蜜素时的干扰情况,选择合适的干扰消除条件。方法样品经涡旋离心提取上清液后,比较不同色谱柱及亚硝酸钠用量的干扰情况,最终选择加入1mL亚硝酸钠,用DB-624(60 m×0.32 mm×1.8μm)色谱柱进行测定。结果在0.01~0.50 mg/mL范围内有良好的线性关系,相关系数为0.9999,相对标准偏差为3.4%和6.2%(n=6),回收率为90%和111%。结论本研究中干扰得到消除,达到了检测要求。

Objective To compare the interference of gas chromatograph in the determination of cyclamate in steamed bread under different conditions,select the appropriate interference cancellation conditions.Methods The sample was eddied,centrifugated and supematant extracted,the interference conditions under different columns and sodium nitrite dosages were compared,then the sample was determined with adding 1 mL of sodium nitrite dosage and using column of DB-624(60 m×0.32 mm×1.8μm).Results The content had a good linear relationship in the range 10-500μg/mL,the correlation coefficient was 0.9999,the relative standard deviations were 3.4%and 6.2%(n=6),the rates of recovery were 90%and 111%.Conclusion The interference is eliminated,and the detection requirements are met.