LC-AJS ESI-MS/MS测定酒中七种甜味剂和氨基甲酸乙酯  

Determination of Seven Sweeteners and Ethyl Carbamate in Wine byLC-AJSESI-MS/MS

作　　者：孙莉 周玉 余义 唐艳荣 SUN Li;ZHOU Yu;YU Yi;TANG Yanrong(Yellow Crane Tower Liquor Co.,Ltd.,Wuhan 430050;Hubei Xinjia Testing Technology Co.,Ltd.,Xianning 43700)

机构地区：[1]黄鹤楼酒业有限公司,武汉430050 [2]湖北信嘉检测科技有限公司,咸宁437000

出　　处：《食品工业》2023年第10期300-305,共6页The Food Industry

摘　　要：通过对液相色谱和质谱条件进行优化,建立液相色谱质谱法同时分离测定酒中甜蜜素、安赛蜜、糖精钠、阿斯巴甜、纽甜、三氯蔗糖、阿力甜、氨基甲酸乙酯的方法。采用ZORBAX Eclipse Plus C18色谱柱(150mm×2.1 mm,1.8μm)进行分离;流动相为甲醇(B)-0.1%乙酸溶液(A),梯度洗脱;流速0.15 mL/min;柱温40℃。结果显示:酒样经0.22μm有机滤膜过滤后备用,在优化的色谱条件下,7种甜味剂和氨基甲酸乙酯分离效果好;定性检出限(r_(SN)=3)为0.005 mg/kg;定量检出限(r_(SN)=10)为0.010 mg/kg;7种甜味剂的线性范围为5~50μg/L,线性线性相关系数均大于0.99;重复性和再现性相对偏差为0.4%~9.4%(n=6);加标浓度,甜味剂为10,25和45μg/kg,氨基甲酸乙酯为300,400和500μg/kg,样品回收率为80%~120%。该前处理方法操作简单快速,为酒中甜蜜素、安赛蜜、糖精钠、阿斯巴甜、纽甜、三氯蔗糖、阿力甜、氨基甲酸乙酯的提取分离及检测提供了有效的方法。Optimize the conditions of liquid chromatography and mass spectrometry,and establish a method for the simultaneous determination of sodium cyclamate,acesulfame,sodium saccharin,Aspartame,neotame,sucralose,alitame and Ethyl carbamate in wine by liquid chromatography-mass spectrometry.A Zorbax Eclipse Plus Cis column(150 mmx2.1 mm,1.8μm)was used for separation.The mobile phase was methanol(B)-0.1%acetic acid solution(A),gradient elution,flow rate 0.15 mL/min,and column temperature 40℃.The results showed that the liquor samples were filtered by 0.22μm organic filter membrane,and the separation eficiency of the seven sweeteners and Ethyl carbamate was good under the optimized chromatographic conditions.The qualitative detection limit(r_(SN)=3)was 0.005 mg/kg,the quantitative detection limit(r_(SN)=10)was 0.010 mg/kg,the linear range was 5-50μg/L for the seven sweeteners,and the linear correlation coefficients were all greater than 0.99.The relative deviation of repeatability and reproducibility was 0.4%-9.4%(n-6).The standard concentration of sweetener was 10,25 and 45μg/kg,and the Ethyl carbamate was 300,400 and 500μg/kg.The recovery rate was 80%-120%.This method was simple and rapid,and it provided an effective method for the extraction,separation and determination of cyclamate,acesulfame,sodium saccharin,Aspartame,neotame,sucralose,alitame and Ethyl carbamate in wine.

关 键 词：液相色谱质谱法 酒类 甜味剂 氨基甲酸乙酯 方法学研究 

分 类 号：TS261.7[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]