市售馒头中甜蜜素含量调查分析

Analysis of the Content of Sodium Cyclamate in Commercially Steamed Bread

目的:采用液相色谱质谱法测定馒头中的甜蜜素含量,对市售馒头中甜蜜素的添加情况进行调查分析,为市场监管开辟路径。方法:以《食品安全国家标准食品中环己基氨基磺酸盐的测定》(GB 5009.97—2023)第三法液质法为基础,通过优化流动相和样品前处理,建立液相色谱质谱法测定馒头中甜蜜素。以购自超市及早餐店的50份馒头为研究对象,测定其甜蜜素的添加情况。结果:所建立的甜蜜素检测方法在2.0~200.0 ng·mL^(-1)线性良好,相关系数r=0.9999。在馒头样品中添加10.0 ng·mL^(-1)、20.0 ng·mL^(-1)、100.0 ng·mL^(-1)3个浓度水平,加标回收率为105.36%~110.86%,相对标准偏差为1.01%~2.31%。购自超市的20份馒头样品,甜蜜素检出率为0;购自早餐店的30份馒头样品,甜蜜素检出率23.33%,最高检出值1.6658 g·kg^(-1)。结论:优化后的方法能准确、高效地测定馒头中甜蜜素,检测结果说明市售馒头生产加工过程中存在违规使用甜蜜素情况。

Objective:The content of sodium cyclamate in steamed bread was determined by liquid chromatography-mass spectrometry,and the addition of sodium cyclamate in steamed bread on the market was investigated and analyzed to open up a path for market supervision.Method:Optimizing the conditions of flow phase and sample pretreatment to establish a method for the determination of sodium cyclamate in steamed bread by LC-MS.Taking steamed bread from supermarket and breakfast shop as the research object to analyze the sodium cyclamate content by the constructed method.Result:The linearity of sodium cyclamate was good in the range of 2.0~200.0 ng·mL^(-1),and the correlation coefficient was r=0.9999.At three spiked concentration levels of 10.0 ng·mL^(-1),20.0 ng·mL^(-1),100.0 ng·mL^(-1)in steamed bread,the recoveries of sodium cyclamate were 105.36%~110.86%,and the relative standard deviation were 1.01%~2.31%.The result shows the sodium cyclamate was not detected in the 20 steamed bread purchased by the supermarket.The detection rate of sodium cyclamate was 23.33%in the 30 steamed bread purchased by the breakfast shop,the maximum detection concentration was 1.6658 g·kg^(-1).Conclusion:The optimized method is accurate and efficient,and some producers use cyclamate in violation of regulations in the production and processing of steamed bread.