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超高效液相色谱-三重四极杆/复合线性离子阱质谱法检测白酒中甜味剂 被引量:3

Determination of Sweeteners in Baijiu by Ultra Performance Liquid Chromatography-Triple Quadrupole Composite Linear Ion Trap Mass Spectrometry
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摘要 目的:基于超高效液相色谱三重四极杆复合线性离子阱质谱联用技术,建立白酒中甜味剂安赛蜜、糖精钠、甜蜜素、阿斯巴甜、纽甜、阿力甜、三氯蔗糖、爱得万甜及麦芽糖醇的检测方法。方法:样品经热水浴除杂,经phenomenex kinetex F5色谱柱分离,乙腈和0.1%甲酸5 mmol/L乙酸铵水溶液为流动相,梯度洗脱,质谱分析采用多反应监测-信息关联采集-增强子离子扫描模式。结果:9种甜味剂在0.025~1.000 mg/mL内线性关系良好(R≥0.995),检出限(Limit of Detection,LOD)在0.001~0.048 mg/kg,定量限(Limit of Quantification,LOQ)为0.004~0.160 mg/kg。在0.25 mg/kg、0.50 mg/kg、1.00 mg/kg 3个不同水平浓度进行加标实验,平均回收率为80.9%~110.1%,相对标准偏差为3.78%~11.80%(n=6)。结论:本方法前处理简单、快速,重复性、稳定性、精密度及灵敏度均较好,且在低浓度时出现判定假阳性概率低,适用于白酒中安赛蜜、糖精钠、甜蜜素、阿斯巴甜、纽甜、阿力甜、三氯蔗糖、爱得万甜及麦芽糖醇的检测。 Objective:Based on the ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry,the detection methods of acesulfame,saccharin sodium,cyclamate,aspartame,neotame,alite,sucralose,aldermentaine and maltitol were established.Method:The samples were removed by hot water bath and separated by phenomenex kinetex F5 chromatographic column.Acetonitrile and 0.1%formic acid 5 mmol/L ammonium acetate aqueous solution were used as mobile phase.Gradient elution and mass spectrometry were analyzed by multi reaction monitoring information correlation collection enhancer ion scanning mode.Result:The linearity of 9 sweeteners was good in the range of 0.025~1.000 mg/mL(R≥0.995),the detection limit(LOD)was 0.001~0.048 mg/kg,and the quantitative limit(LOQ)was 0.004~0.160 mg/kg.The standard addition experiments were carried out at three different concentrations of 0.25 mg/kg,0.50 mg/kg and 1.00 mg/kg.The average recovery was 80.9%~110.1%,and the relative standard deviation was 3.78%~11.80%(n=6).Conclusion:The method is simple,rapid,repeatable,stable,accurate and sensitive,and has low false positive probability at low concentration.It is suitable for the detection of acesulfame,saccharin sodium,cyclamate,aspartame,neotame,alite,sucralose,aldermentaine and maltitol in Baijiu.
作者 倪小龙 吴金凯 陆雪梅 梅婕 张温清 周萍 NI Xiaolong;WU Jinkai;LU Xuemei;MEI Jie;ZHANG Wenqing;ZHOU Ping(Xuancheng Centre for Food and Drug Control,Xuancheng 242000,China;Anhui Xuanjiu Group Co.,Ltd.,Xuancheng 242000,China)
出处 《食品安全导刊》 2022年第20期65-70,共6页 China Food Safety Magazine
基金 安徽省市场局科技项目“超高效液相色谱三重四级杆与离子阱联用(UPLC-QTRAP)同时检测白酒中九种甜味剂”(2020MK022)。
关键词 超高效液相色谱-三重四极杆/复合线性离子阱质谱 白酒 甜味剂 ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry Baijiu sweetener
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