超高效液相色谱串联质谱同时测定酒类产品中多种人工合成甜味剂

建立超高效液相色谱-电喷雾电离串联质谱（ultra performance liquid chromatography-electro spray ionizationtandem mass spectrometry，UPLC-ESI-MS-MS）同时测定酒类产品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜人工合成甜味剂的分析方法。方法采用ZORBAX Eclipse XDB-C18柱（100 mm×4.6 mm，1.8 μm）色谱柱，柱温50 ℃。流动相由A（甲醇）和B（体积分数0.1%甲酸和20 mmol/L甲酸铵溶液，pH 4.0）组成，流速为0.5 mL/min，梯度洗脱。在ESI负离子模式下，采用多反应监测模式进行测定，可以在12.5 min内完成7 种人工合成甜味剂的检测。安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜在10～5 000 μg/L范围内有良好的线性关系，相关系数大于0.999。安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜检出限分别为4、6、4、8、4、4、2 μg/L，回收率在88.3%～98.3%之间，相对标准偏差为2.1%～6.7%。该方法快速、准确，灵敏度高，适用于酒类产品中低含量人工合成甜味剂的测定。

Simultaneous Determination of Synthetic Sweeteners in Liquor Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESIMS-
MS) method was developed for the simultaneous determination of seven synthetic sweeteners, acesulfame-K, sodium
saccharin, sodium cyclamate, sucralose, aspartame, alitame and neotame, in liquor products. ZORBAX Eclipse XDB-C18
column (100 mm × 4.6 mm, 1.8 μm) chromatographic column was used, and the solvent system was composed of mobile
phase A (methanol), and mobile phase B (0.1% formic acid and 20 mmol/L ammonium formate in water, pH 4.0). The flow
rate was 0.5 mL/min for gradient elution, and the column temperature was held at 50 ℃. In the ESI negative ion mode,
multiple reaction monitoring (MRM) was used for quantitation. The 7 kinds of artificial sweeteners were successfully
detected within 12.5 min. These sweeteners showed good linear relationships in the range of 10–5 000 μg/L with correlation
coefficients larger than 0.999. The limits of detection (LODs) for acesulfame-K, saccharin sodium, sodium cyclamate,
sucralose, aspartame, alitame and neotame were 4, 6, 4, 8, 4, 4 and 2 μg/L, respectively, and recovery rates for spiked
samples ranged from 88.3% to 98.3%, with relative standard deviations between 2.1% and 6.7%. A rapid, accurate and
sensitivity method has been developed in this study and this method has been successfully applied to the determination of
synthetic sweeteners at low levels in liquor products.