分散液液微萃取结合气相色谱-四极杆/飞行时间质谱法同时测定饮料中21种邻苯二甲酸酯

Simultaneous determination of 21 kinds of phthalic acid esters in beverage by dispersive liquid-liquid micro-extraction with gas chromatography-high resolution quadrupole time-of-flight mass spectrometry

中文关键词:  分散液液微萃取  气相色谱-四极杆/飞行时间质谱法  饮料  邻苯二甲酸酯

英文关键词:dispersive liquid-liquid micro-extraction  gas chromatography-high resolution quadrupole time-of-flight mass spectrometry  beverage  phthalic acid esters

中文摘要:

      目的 建立分散液液微萃取(dispersive liquid-liquid microextraction, DLLME)结合气相色谱-四极杆/飞行时间质谱法(gas chromatography high resolution quadrupole time of flight mass spectrometry, GC-Q-TOF/MS)同时测定饮料中21种邻苯二甲酸酯(phthalic acid esters, PAEs)的分析方法。方法 样品经正丙醇分散, 四氯化碳提取, 氮气吹干, 正己烷复溶。在该优化的色谱及质谱条件下, 采用电子轰击离子源, 全扫描方式采集数据, 根据碎片离子的精确质量数定性定量。结果 21种邻苯二甲酸酯在5.0~1000.0 μg/L范围内呈良好线性关系, 相关系数r均大于0.9985, 平均回收率为70.1%~109.9%, 检出限为1.0~5.0 μg/L, 定量限为3.0~16.0 μg/L, 相对标准偏差为3.02%~6.68%。结论 该方法具有操作简便、高效快速、回收率高、灵敏度高等优点, 可用于分析测定饮料中的21种邻苯二甲酸酯。

英文摘要:

      Objective To establish a method for determination of 21 kinds of phthalic acid esters (PAEs) in beverage by dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-high resolution quadrupole time-of-flight mass spectrometry (GC-Q-TOF/MS). Methods Samples were extracted with N-propanol and carbon tetrachloride, then dried by nitrogen and dissolved with hexane. Under the optimized chromatographic and mass spectral conditions, the result data was obtained with electron impact ion source (EI) and total scan mode. Accurate qualitatuve and quantitative analysis based on the exact mass number of fragment ions were achieved. Results The calibration curves of 21 kinds of PAEs showed good linearities within the concentrations of 5.0-1000.0 μg/L (r＞0.9985). The corresponding average recoveries were in the range of 70.1%-109.9%. Futher, the limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 1.0?5.0 μg/L and 3.0?16.0 μg/L, respectively. The relative standard deviations (RSDs) were 3.02%?6.68%. Conclusion This method shows the advantages of simple operation, high efficiency and time-saving, with a high recovery rate as well as a high sensitivity. The method is suitable for the determination of 21 phthalates in beverages.