超高效液相色谱串联质谱法测定白酒中8种甜味剂和氨基甲酸乙酯  

Determination of 8 sweeteners and ethyl carbamate in Baijiu by ultra performance liquidchromatography-tandem mass spectrometry

作　　者：张建辉 禹琼 王鑫 胡绍武 孙燕平 黄静 张玉 陈喜栋 ZHANG Jianhui;YU Qiong;WANG Xin;HU Shaowu;SUN Yanping;HUANG Jing;ZHANG Yu;CHEN Xidong(Shedian Wine Co.,Ltd.,Nanyang 473300,China)

机构地区：[1]赊店老酒股份有限公司,河南南阳473300

出　　处：《中国酿造》2024年第12期266-270,共5页China Brewing

基　　金：河南省豫酒振兴创新重大科技专项项目(181100211400)。

摘　　要：该实验建立了一种超高效液相色谱串联质谱(UPLC-MS/MS)仪测定白酒中氨基甲酸乙酯(EC)和8种甜味剂(三氯蔗糖、糖精钠、甜蜜素、安赛蜜、阿斯巴甜、纽甜、阿力甜、甜菊糖苷)的方法。白酒样品经0.22μm有机滤膜过滤后直接进样供质谱检测,使用Agilent ZORBAX RRHD Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8μm)分离,以甲醇-0.1%乙酸水溶液作为流动相梯度洗脱,柱温40℃,流速0.35 m L/min,采用正、负离子模式切换检测,进样时间9 min。结果表明,9种待测物在质量浓度2~500μg/L范围内有良好的线性关系,相关系数(R^(2))均>0.997,检出限为0.1~0.4μg/L,在100μg/L加标水平下,回收率在92.6%~108.7%,相对标准偏差(RSD)<2%。该检测方法前处理简单、重现性好、灵敏度高、分析速度快,可用于白酒中氨基甲酸乙酯和8种甜味剂的快速检测和日常监测。A method was established for the determination of ethyl carbamate(EC)and 8 kinds of sweeteners(sucralose,saccharin sodium,cyclamate,acesulfame potassium,aspartame,neotame,alitame,stevioside)in Baijiu by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The Baijiu samples were filtered by 0.22μm organic filter film and directly injected for mass spectrometry,separated using Agilent ZORBAX RRHD Eclipse Plus C18 column(100 mm×2.1 mm,1.8μm)with gradient elution of methanol and 0.1%acetic acid aqueous solution,column temperature 40℃and flow rate 0.35 ml/min,and detected by switching between positive and negative ion modes using ULPC-MS/MS.The injection time was 9 min.The results showed that 9 tested substances had a good linear relationship in the range of 2-500μg/L,the correlation coefficients(R^(2))were all greater than 0.997,the detection limits were 0.1-0.4μg/L,and the recoveries were 92.6%-108.7%under the spiked levels of 100μg/L,and the relative standard deviations(RSD)were lower than 2%.The detection method had the advantages of simple pretreatment,good reproducibility,high sensitivity and fast analysis,and could be used for rapid detection and daily monitoring of EC and 8 kinds of sweeteners in Baijiu.

关 键 词：UPLC-MS/MS 白酒 甜味剂 氨基甲酸乙酯 检测 

分 类 号：TS261.7[轻工技术与工程—发酵工程] TS262.33[轻工技术与工程—食品科学与工程]