液相色谱串联质谱法测定冷冻饮品中环己基氨基磺酸钠

Determination of Sodium Cyclamate in Frozen Drinks by Liquid Chromatography–Tandem Mass Spectrometry

建立了液相色谱～串联质谱测定冷冻饮品中环己基氨基磺酸钠的方法。冷冻饮品经净化、冷冻离心后用水稀释定容，采用C18色谱柱（50mm×2．1mm，1．7μm），以乙腈-0．01mol／L乙酸铵缓冲溶液为流动相，电喷雾离子源负离子模式（MRM）定性、定量测定环己基氨基磺酸钠。环己基氨基磺酸钠的质量浓度在2—1000μg／L范围内与峰面积呈线性关系，相关系数，=0．9999，方法的定量限为0．02mg／kg。在10—100μg／L范围内，3水平加标回收率为87．5％～101．8％，测定结果的相对标准偏差为3．0％（H=6）。该方法净化效果好，灵敏度高，能快速完成冷冻饮品中环己基氨基磺酸钠的测定。

A Liquid chromatography-tandem mass spectrometry method for determination of sodium cyclamate in frozen drinks was developed. The frozen drinks sample was purified, diluted with ultra-pure water, then the sodium cyclamate in the sample was detected by LC-MS/MS in MRM mode using C18 column（50 mm×2.1 mm, 1.7 μm） and acetonitrile-0.02 mol/L as mobile phase. The mass concentration of sodium cyclamate had good linear relationship with peak area in the range of 2-1 000 μ g/L, with the correlation coefficient of 0.999 9, and the limit of quantification was 0.02 mg/kg. The recoveries of sodium cyclamate spiked in sample at three levels were 87.5 %-101.8%, and the relative standard deviation was 3.0%（n=6）. The method is sensitive and can simultaneously complete quantification analysis of sodium cyclamate in frozen drinks.