白酒和调香剂中4种人工合成甜味剂的UPLC-MS-MS测定  

Simultaneous UPLC-MS/MS Determination of Four Artificial Sweeteners in Luzhou Flavor Liquor and Flavoring Agents

作　　者：郭莹莹[1] 乔善磊[1] 李磊[1] 周靖平[1] 戴金凤[1] 

机构地区：[1]南京医科大学公共卫生学院,江苏南京210029

出　　处：《食品科学》2010年第14期245-249,共5页Food Science

摘　　要：目的:建立白酒及调香剂中人工合成的非营养性甜味剂--甜蜜素、糖精钠、安赛蜜、阿斯巴甜的超高效液相色谱-串联质谱检测法(UPLC-MS-MS),并用于市售白酒和调香剂中4种甜味剂的测定。方法:采用WatersACQUITY UPLC BEH C18色谱柱(50mm×2.1mm,1.7μm),以乙腈-0.01g/100mL氨水为流动相,梯度洗脱,流速0.2mL/min,待测物经电喷雾离子源负离子化后,用三重四级杆串联质谱仪的多反应离子监测(MRM)方式进行定量分析。结果:4种甜味剂质量浓度在10～1000μg/L范围内均与峰面积呈良好线性关系(r≥0.997),检出限为0.03～0.35μg/L,平均加标回收率在75.2%～115.3%之间,相对标准偏差在8%以内。市售白酒和调香剂中甜蜜素、糖精钠和阿斯巴甜的含量分别为0～287、0～67.2、0～104.8μg/L,样品中没有发现安赛蜜。结论:本方法快速简便、检出限低,适合于白酒和调香剂中微量甜味剂的同时检测。Objective： To establish a UPLC-MS/MS method for the simultaneous determination of four artificial nonnutritive sweeteners,cyclamate,saccharin,acesulfame-K and aspartame in Luzhou flavor liquor and flavoring agents.Methods： The chromatographic separation was achieved on a Waters ACQUITY UPLC BEH C18 column （50 mm × 2.1 mm,1.7μm） using acetonitrile/0.01% ammonia water as mobile phase in the gradient elution mode at a flow rate of 0.2 mL/min.Electrospray ionization （ESI） in the negative ion mode followed by triple quadrupole mass spectrometric analysis in the multiple reaction monitoring mode （MRM） was used for quantification.Results： The concentrations of these four sweeteners ranging from 10 to 1000μg/L had good linear relationship with the peak area.The limits of detection （LODs） ranged from 0.03 to 0.35μg/L.The average recoveries for them were between 75 .2% and 115.3% in Luzhou flavor liquor sample NO and between 100.3% and 116.1% in flavoring agent sample W3 and the relative standard derivations were all within 8%.The contents of cyclamate,saccharin and aspartame in 10 Luzhou flavor liquor samples and 5 flavoring agent samples tested in this study were found to range from 0 to 287 μg/L,from 0 to 67.2 μg/L and from 0 to104.8 μ g/L,respectively,but none of them was found to contain acesulfame-K.Conclusions： The method is of simplicity and presents lower LODs than other methods reported previously.Thus it is more suitable for simultaneous determination of trace amount of sweeteners in distillate spirit.

关 键 词：白酒 调香剂 超高效液相色谱-串联质谱 人工合成甜味剂 

分 类 号：TS207.3[轻工技术与工程—食品科学]