发酵酒中甜蜜素的确证技术分析及解决方案  

Technical analysis and solutions for the sodium cyclamate confirmation in fermented wine

作　　者：张书芬 张爱芝 忻璐琰 芦童 邢家溧 王志强 刘艳 励丹 何怡 袁伟 ZHANG Shufen;ZHANG Aizhi;XIN Luyan;LU Tong;XING Jiali;WANG Zhiqiang;LIU Yan;LI Dan;HE Yi;YUAN Wei(Ningbo Academy of Product and Food Quality Supervision and Inspection(Ningbo Fiber Inspection Institute),Ningbo 315040,China)

机构地区：[1]宁波市产品食品质量检验研究院(宁波市纤维检验所),浙江宁波315040

出　　处：《中国酿造》2021年第8期186-190,共5页China Brewing

基　　金：食品安全国家标准立项计划(spaq-2019-035)。

摘　　要：为了解决发酵酒中甜蜜素测定的基质干扰和离子丰度比偏差不能满足液相色谱-质谱法的要求的问题,将发酵酒样品挥去酒精,经水稀释后,以甲醇-5 mmol/L甲酸铵为流动相,以BEH C18色谱柱(100 mm×2.1 mm,1.7μm)进行分离,采用多反应监测(MRM)正负离子同时采集模式分析,当甜蜜素含量≥2 mg/kg时,稀释后进行确认,当甜蜜素含量<2 mg/kg时,采用WAX固相萃取小柱净化后进行确认。经过方法学验证,该方法线性关系良好,相关系数R2为0.9992,在3个添加水平条件下的加标回收率为82%~109%,测定结果的相对标准偏差(RSD)为2.2%~8.6%(n=6),方法检出限为0.03 mg/kg,定量限为0.1 mg/kg。该方法准确、稳定性好,从实际检测出发较好地解决了发酵酒中甜蜜素定性困难问题。In order to solve the problem that the matrix interference and ion abundance ratio deviation of sodium cyclamate determination could not meet the requirements of liquid chromatography-mass spectrometry method in fermented wine,fermented wine samples were evaporated from alcohol,diluted with water,separated by BEH C18 column(100 mm×2.1 mm,1.7μm)with methanol-ammonium formate(5 mmol/L)as mobile phase,and analyzed by multiple reaction monitoring(MRM)positive/negative ion simultaneous acquisition mode.The sodium cyclamate was confirmed after dilution when the contents of sodium cyclamate were≥2 mg/kg,and confirmed after purification with WAX solid phase extraction cartridge when the contents of sodium cyclamate were<2 mg/kg.Through methodological verification,the method had a good linear relationship with correlation coefficient R20.9992,the recovery rate of standard addition under the conditions of 3 addition levels was 82%-109%,and the relative standard deviation(RSD)of the measurement results was 2.2%-8.6%(n=6).The detection limit of the method was 0.03 mg/kg,and the quantification limit was 0.1 mg/kg.The method was accurate and stable,and proceeding from the actual detection,the problem of qualitative difficulty of sodium cyclamate in fermented wine was solved.

关 键 词：发酵酒 甜蜜素 超高效液相色谱-串联质谱 基质效应 确证 

分 类 号：TS261.7[轻工技术与工程—发酵工程]