饮料中35种添加剂的超高效液相色谱/四级杆-飞行时间质谱筛查法

Screening of 35 kinds of additives in beverages by ultra high performance liquid chromatography coupled with quadrupole-time-of-flight

目的:建立超高效液相色谱-四级杆-飞行时间质谱(ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry,UPLC-Q-TOF MS)快速检测饮料中35种添加剂(3种防腐剂、5种甜味剂和27种色素)的分析方法。方法:样品用乙腈-水(8∶2)提取后,采用XBridge Peptide BEH C18色谱柱(100 mm×2.1 mm,3.5μm)分离,以乙腈-0.025%甲酸水溶液(含10 mmol/L的甲酸铵)为流动相,梯度洗脱,Q-TOF MS电喷雾正、负离子模式分析检测。在全扫描采集模式下,以准分子离子峰的峰面积定量,以化合物的色谱保留时间和精确质量数定性。在Target MS/MS采集模式下,通过碎片离子的精确质量数进一步确证化合物。结果:35种添加剂在0.002~100 mg/kg范围内具有较好的线性关系,相关系数均大于0.99,其定量限为0.01~10 mg/kg,添加回收率在70.5%~110.6%范围内,相对标准偏差(RSD)均小于2.8%~11.5%(n=6)。结论:该方法简便、快速、灵敏,适用于饮料中多类添加剂的同时检测。

Purpose：An analytical method was established for the simultaneous determination of 35 additives（3 pigments,5 sweeteners and 27 colours in beverages by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry（UPLC-Q-TOF MS）.Methods：The sample was extracted by acetonitrile–water（8∶2）,and then separated by Bridge Peptide BEH C18（100 mm×2.1 mm,3.5μm）with acetonitrile-0.025% formic acid containing 10 mmol/L ammonium formate as mobile phase under gradient elution.The extract was determined directly by LC-Q TOF MS with electrospray ionization in positive and negative mode.Under full scan acquisition mode,the peak area of excimer ion peak determined the quantitative part,and retention time and accurate masses of the compound determined the qualitative part.The compound was further confirmed by fragment ions accurate mass under Target MS/MS acquisition mode.Results：The method had good linearity（r〉0.99）in the linear range of 0.002~100 mg/kg.The limits of quantification（LOQS） of 35 analytes were between 0.01 mg/kg and10 mg/kg.The recoveries ranged from 70.5%to 110.6%at three spiked levels with relative standard deviations（RSDs）ranged from 2.8%~11.5%.Conclusion：The method is rapid,sensitive and easy to apply,and is suitable for the simultaneous determination of various type additives in beverages.