首页|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

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

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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0.22 μm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,1.8 μm)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 mL/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2~500 μg/L范围内有良好的线性关系,相关系数(R2)均>0.997,检出限为0.1~0.4 μg/L,在100 μg/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.
Determination of 8 sweeteners and ethyl carbamate in Baijiu by ultra performance liquid chromatography-tandem mass spectrometry
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 0.22 µm organic filter film and directly injected for mass spectrometry,separated using Agilent ZORBAX RRHD Eclipse Plus C18 column(100 mm×2.1 mm,1.8 µm)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 2-500 μg/L,the correlation coefficients(R2)were all greater than 0.997,the detection limits were 0.1-0.4 μg/L,and the recoveries were 92.6%-108.7%under the spiked levels of 100 μg/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.

UPLC-MS/MSBaijiusweetenerethyl carbamatedetection

张建辉、禹琼、王鑫、胡绍武、孙燕平、黄静、张玉、陈喜栋

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赊店老酒股份有限公司,河南南阳 473300

UPLC-MS/MS 白酒 甜味剂 氨基甲酸乙酯 检测

2024

中国酿造
中国调味品协会 北京食品科学研究院

中国酿造

CSTPCD北大核心
影响因子:0.759
ISSN:0254-5071
年,卷(期):2024.43(12)