关键词: 白酒, 调香剂, 超高效液相色谱- 串联质谱, 人工合成甜味剂

Abstract:

Objective: To establish a UPLC-MS/MS method for the simultaneous determination of four artificial nonnutritive sweeteners, cyclamate, saccharin, acesulfame-K and aspartame in Luzhou flavor liquor and flavoring agents. Methods: The chromatographic separation was achieved on a Waters ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, 1.7μm) using acetonitrile/0.01% ammonia water as mobile phase in the gradient elution mode at a flow rate of 0.2 mL/min. Electrospray ionization (ESI) in the negative ion mode followed by triple quadrupole mass spectrometric analysis in the multiple reaction monitoring mode (MRM) was used for quantification. Results: The concentrations of these four sweeteners ranging from 10 to 1000μg/L had good linear relationship with the peak area. The limits of detection (LODs) ranged from 0.03 to 0.35μg/L. The average recoveries for them were between 75 .2% and 115.3% in Luzhou flavor liquor sample NO and between 100.3% and 116.1% in flavoring agent sample W3 and the relative standard derivations were all within 8%. The contents of cyclamate, saccharin and aspartame in 10 Luzhou flavor liquor samples and 5 flavoring agent samples tested in this study were found to range from 0 to 287 μg/L, from 0 to 67.2 μg/L and from 0 to104.8μg/L, respectively, but none of them was found to contain acesulfame-K. Conclusions: The method is of simplicity and presents lower LODs than other methods reported previously. Thus it is more suitable for simultaneous determination of trace amount of sweeteners in distillate spirit.

Key words: Luzhou flavor liquor, flavoring agent, UPLC-ESI-MS/MS, artificial sweeteners