UPLC-MS/MS法同时测定白酒中氨基甲酸甲酯和氨基甲酸乙酯  

Simultaneous Determination of Methyl Carbamate and Ethyl Carbamate in Baijiu by UPLC-MS/MS

作　　者：陈艳 刘冲 张国宇 张琴 任伟 张冰雪 CHEN Yan;LIU Chong;ZHANG Guoyu;ZHANG Qin;REN Wei;ZHANG Bingxue(Zunyi Product Quality Inspection and Testing Institute,Zunyi,Guizhou 563000,China)

机构地区：[1]遵义市产品质量检验检测院,贵州遵义563000

出　　处：《酿酒科技》2023年第9期47-52,共6页Liquor-Making Science & Technology

摘　　要：建立同时快速测定白酒中氨基甲酸甲酯(MC)和氨基甲酸乙酯(EC)含量的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。样品无需前处理,直接进样,经Waters Acquity UPLC HSS T3 C18柱(2.1 mm×100 mm,1.8μm)分离,乙腈和0.1%甲酸水作为流动相,以0.2 mL/min的流速梯度洗脱,在UPLC-MS/MS多反应监测(MRM)正模式检测条件下,对MC和EC进行分析。结果表明,MC和EC在10~200μg/L浓度范围内,线性关系良好,相关系数R2分别为0.9994和0.9996,两者定量限(LOQ)分别为8.5μg/L和7.6μg/L,MC加标回收率为76.29%~85.73%,RSD为3.8%~5.5%,EC加标回收为87.73%~98.81%,RSD为2.8%~3.0%,该方法高效、准确、稳定、灵敏度高。检验结果发现,不同类型白酒中均未检出MC,EC均有检出且含量存在显著性差异。A rapid UPLC-MS/MS method for simultaneous determination of the content of methyl carbamate(MC) and ethyl carbamate(EC) in Baijiu was established.The samples were injected directly without pretreatment.The analytes were separated by Waters Acquity UPLC HSS T3 C18 column(2.1 mm×100 mm,1.8 μm),gradient eluted by acetonitrile and 0.1 % formic acid aqueous solution at the flow rate of 0.2 m L/min,and then analyzed by UPLC-MS/MS under multi reaction monitoring(MRM) mode.The results showed that MC and EC demonstrated good linearity within the concentration range of 10 μg/L to 200 μg/L.The linear correlation coefficient of MC was 0.9994,the limit of quantification(LOQ) was 8.5 μg/L,the spiked recovery rate was between 76.29 % and85.73 %,and the relative standard deviation(RSD) was between 3.8 % and 5.5 %.The linear correlation coefficient of EC was0.9996,the limit of quantification(LOQ) was 7.6 μg/L,the spiked recovery rate was between 87.73 % and 98.81 %,and the relative standard deviation(RSD) was between 2.8 % and 3.0 %.The method was efficient,accurate,stable,and sensitive.The results showed that MC was not detected,while EC was detected in various types of Baijiu,and its content had significant difference.

关 键 词：UPLC/MS-MS 氨基甲酸甲酯 氨基甲酸乙酯 白酒 

分 类 号：TS262.3[轻工技术与工程—发酵工程] TS261.7[轻工技术与工程—食品科学与工程]