超高效液相色谱-串联质谱法检测白酒中9种甜味剂含量

Simultaneous determination of 9 kinds of sweeteners in liquor by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  甜味剂  超高效液相色谱-串联质谱法  白酒  检测方法

英文关键词:sweeteners  ultra performance liquid chromatography-tandem mass spectrometry  liquor  detection method

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测白酒中爱德万甜、甜菊糖苷等9种甜味剂的分析方法。方法 白酒样品经水浴加热除去乙醇、定容、过0.22 μm滤膜后, 采用体积分数0.1%甲酸水溶液和纯甲醇作为流动相进行梯度洗脱, 色谱柱选用迪马Endeavorsil C18 (100 mm×2.1 mm, 1.8 μm)色谱柱, 质谱(ESI+、ESI-)采用多反应监测模式(multiple response monitoring, MRM), 对9种甜味剂的定量、定性离子进行检测。结果 本方法在10 min内可完成9种目标化合物的分离分析。9种甜味剂分别根据检出限在20、50、100、500 μg/L等2个添加水平的回收率范围为84.8%~102.4%, 相对标准偏差范围3.6%~8.3%(n=6), 各个甜味剂组分方法定量限范围1.0~ 15 μg/kg。结论 该方法简单快、快速、结果准确、灵敏度高, 适合测定白酒中爱德万甜、甜菊糖苷等9种甜味剂。

英文摘要:

      Objective To establish a method for simultaneous determination of 9 sweeteners in liquor by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The liquor samples were heated in water bath to remove ethanol before adding water making constant volume. The solution passed the 0.22 μm filter membrane and was separated on a reversed phase using a gradient elution program of 0.1% (V/V) formic acid aqueous solution and menthol solution through Endeavorsil C18 (100 mm×2.1 mm, 1.8 μm) and detected by MS/MS under multiple reaction monitoring (MRM) mode. Using MS/MS (ESI+, ESI-) with multiple reactions monitoring (MRM), identification of the major components of 9 sweeteners was performed based upon the intensities of fragments. Results In this method, 9 target compounds were isolated and analyzed within 10 min. The recovery rates of the 9 sweeteners were 84.8% to 102.4% according to the detection limits of 20, 50, 100, 500 μg/L. The relative standard deviations (RSDs) were less than 8.3% (n=6), and the limits of quantitation (LOQ) for the 9 sweeteners were 15 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting 9 sweeteners in wine.