超高效液相色谱-串联质谱快速测定饮料中甜蜜素的方法探讨

Rapid determination of sodium cyclamate in beverage by ultra high performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法快速测定饮料中甜蜜素的方法。方法样品经Agilent Eclipse plus C18色谱柱分离,流动相为乙腈-乙酸铵溶液(0.02 mol/L),电喷雾串联质谱多反应监测模式测定,外标法定量。结果甜蜜素在测定的范围内线性关系良好(r=0.9990),方法的检出限为0.2μg/L(3S/N)。在加标水平为1、10、100μg/L时,方法的回收率为94.3%~110%,相对标准偏差(n=6)为0.29%~2.42%。结论该方法对样品无需衍生化,前处理简单,分析时间短,选择性好,灵敏度高,适用于甜蜜素的快速定性定量检测。

[ Objective ] To develop a new analytical method for the rapid determination of sodium cyclamate in beverage by ultra high performance liquid chromatography-tandem mass spectrometry （LC-MS/MS）. [Methods] The samples were separated on an Agilent Eclipse plus C18 column and analyzed by LC-MS/MS under muhiple reaction monitoring mode via positive eleetrospray ionization, with the mobile phase of acetonitrile-ammonium acetate solution （0.02 tool/L）. The quantitation analysis was carried out by the matrix-matched external standard calibrations. [ Results ] The method showed excellent linearities （r=0.999） for the sodium cyclamate in a certain concentration range. The detection limit was 0.2 p^g/L （3S/N）. The recoveries at three added standard levels of 1, 10, and 100 Ixg/L were between 94.3% and 110%, and the relative standard deviations （n =6） were 0.29%-2.42%. [Conclusion] The method has the advantages of sample without derivatization, simple pretreatment, short analysis time, good selectivity, high sensitivity, which is suitable for rapid qualitative and quantitative determination of sodium cyclamate.