超高效液相色谱串联质谱法快速测定白酒中痕量甜味剂

doi:10.7506/spkx1002-6630-201320049

食品科学

超高效液相色谱串联质谱法快速测定白酒中痕量甜味剂

胡强，王延云，李超豪，杨春林，吴卫，向乐曦

1.乐山市产品质量监督检验所，四川乐山 614000；2.乐山师范学院化学与生命科学学院，四川乐山 614000

出版日期:2013-10-25 发布日期:2013-09-28

Rapid Determination of Trace Sweeteners in Distilled Spirit by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

HU Qiang，WANG Yan-yun，LI Chao-hao，YANG Chun-lin，WU Wei，XIANG Le-xi

Online:2013-10-25 Published:2013-09-28

摘要/Abstract

摘要：

建立同时、快速测定白酒中4种痕量甜味剂(安赛蜜、糖精钠、甜蜜素、阿斯巴甜)的超高效液相色谱-串联质谱(UPLC-MS-MS)分析方法。白酒样品超声脱气后直接进样，经超高效液相色谱(UPLC)快速分离，采用电喷雾负离子(ESI-)、多反应监测模式(MRM)进行质谱分析，实现对目标物的定性和外标法定量。结果表明：4种甜味剂在1.2min内完全分离，相关系数大于0.996，安赛蜜、糖精钠、甜蜜素、阿斯巴甜的方法检出限(LOD)分别为0.5、1.5、1.0μg/L和0.6μg/L；平均回收率分别为92.5%～98.7%、92.3%～96.1%、93.1%～97.3%和94.5%～99.4%，相对标准偏差(RSD)分别为1.0%～1.9%、1.4%～1.9%、1.1%～1.8%、0.9%～1.2%。该方法快速、简单、准确、灵敏，适合于白酒中痕量甜味剂的快速筛查和检测。

关键词: 超高效液相色谱-串联质谱, 白酒, 甜味剂, 痕量

Abstract:

A method for the determination of four trace sweeteners (acesulfame-K, saccharin sodiuma, sodium cyclamate,
and aspartame) has been established using ultra performance liquid chromatography-tandem mass spectrometry
(UPLC-MS-MS). Four sweeteners in distilled spirit samples were separated on UPLC after ultrasonic degassing.
Electrospray ionization (ESI) was applied for MS analysis in the negative ion mode and quantification was performed
in the multiple-reaction-monitoring mode (MRM) through external calibration. Four sweeteners were completely separated
within 1.2 min with good linearity (r ＞ 0.996). The limits of detection (LOD) for aspartame, sodium cyclamate,
saccharin sodiuma and acesulfame-K were 0.5, 1.5, 1.0 μg/L and 0.6 μg/L, respectively. Their recovery rates were
92.5%–98.7%, 92.3%–96.1%, 93.1%–97.3% and 94.5%–99.4% with relative standard deviation (RSD) of 1.0%–1.9%,
1.4%–1.9%, 1.1%–1.8% and 0.9%–1.2%. This method proved to be rapid, simple, accurate and suitable for the screening
and detection of trace sweeteners in distilled spirit.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS), distilled spirit, sweetener, trace

胡强，王延云，李超豪，杨春林，吴卫，向乐曦. 超高效液相色谱串联质谱法快速测定白酒中痕量甜味剂[J]. 食品科学, doi: 10.7506/spkx1002-6630-201320049.

HU Qiang，WANG Yan-yun，LI Chao-hao，YANG Chun-lin，WU Wei，XIANG Le-xi. Rapid Determination of Trace Sweeteners in Distilled Spirit by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201320049.

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超高效液相色谱串联质谱法快速测定白酒中痕量甜味剂

Rapid Determination of Trace Sweeteners in Distilled Spirit by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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