摘要
为了建立UPLC-MS/MS测定浓香型白酒中5种人造甜味剂的快速定量和定性分析方法,本研究将样品直接加水稀释后,采用高速离心进行净化,以ACQUIYT UPLC^(■)BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)为分析柱,0.05%氨水水溶液和甲醇为流动相进行梯度洗脱分离,选取电喷雾电离源,利用UPLC-MS/MS的多反应监测模式,在同一时间下完成5种甜味剂的筛选,针对疑似检出的阳性物质以触发PICs功能,得到二级质谱图,通过与标准品比对得到匹配度数值作为定性确认。结果表明,甜蜜素、糖精钠、安赛蜜、三氯蔗糖和纽甜5种人造甜味剂在0.01~0.5μg/mL范围内线性关系良好(r^(2)>0.99),方法检出限LOD(S/N=3)为0.107~1.92μg/L,方法定量限LOQ(S/N=10)为0.358~6.39μg/L;空白样品在3个加标水平下的平均回收率为91.3%~117.1%,相对标准偏差(relative standard deviations,RSDs,n=6)为0.42%~6.67%。该检测方法操作简单、成本低、结果准确,可用于白酒中人造甜味剂的检测。
To establish a rapid method for the qualitative and quantitative analysis of 5 kinds of artificial sweeteners in Nongxiang Baijiu by UPLC-MS/MS,the samples were diluted directly with water,and then purified by high-speed centrifugation.ACQUIYT UPLC^(■)BEH C_(18)column(2.1 mm×50 mm,1.7μm)was used for separation,and 0.05%ammonia solution and methanol were used as the mobile phase.An electrospray ionization source was selected for qualitative and quantitative analysis,and the multiple reaction monitoring mode of UPLC-MS/MS was used to scan the 5 sweeteners at the same time.For the suspected positive substances,the PICs function was used to obtain the secondary mass spectra,and the matching degree was obtained by comparing with the standard products for qualitative confirmation.The linear relationship of the 5 kinds of artificial sweeteners was good in the range of 0.01μg/mL to 0.5μg/mL(r^(2)>0.99),the limit of detection(LOD,S/N=3)was between 0.107μg/L and 1.92μg/L,the limit of quantification(LOQ,S/N=10)was between 0.358μg/L and 6.39μg/L,the average spiked recovery rates were from 91.3%to 117.1%,and the relative standard deviations(RSDs,n=6)were between 0.42%and 6.67%.The method is simple,low-cost and accurate,and can be used for the detection of artificial sweeteners in Baijiu.
作者
武艳丽
刘石雪
王秀菊
袁韵
刘永花
禚林娜
WU Yanli;LIU Shixue;WANG Xiuju;YUAN Yun;LIU Yonghua;ZHUO Linna(Shandong Zhongke Xinrui Testing and Inspection Co.Ltd.,Linyi,Shandong 276700,China)
出处
《酿酒科技》
2024年第7期25-32,共8页
Liquor-Making Science & Technology
作者简介
武艳丽(1990-),女,山东临沂人,硕士,制糖工程专业,工程师,研究方向为食品安全检测,E-mail:1010761154@qq.com。
