高效液相色谱-串联质谱法同时测定饮料中8种香豆素类化合物

Simultaneous determination of 8 kinds of coumarins in beverage by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  香豆素  高效液相色谱-串联质谱法  同时测定  饮料

英文关键词:coumarins  high performance liquid chromatography-tandem mass spectrometry  simultaneous determination  beverage

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定饮料中8种香豆素类化合物的分析方法。方法 考察不同实验条件对液体饮料和固体饮料中8种香豆素类化合物的提取效果。以乙腈作为提取溶剂, 经超声提取、冷冻离心分层, 采用C18色谱柱分离, 0.2%甲酸水和乙腈作为流动相梯度洗脱, 在正离子扫描模式下采用电喷雾电离多反应监测模式(multiple reaction monitoring, MRM)进行测定, 基质曲线外标法定量。结果 8种目标物在1~200 μg/L质量浓度范围线性良好, 相关系数(r2)为0.9976~0.9999。对于液体饮料, 方法检出限(limits of detection, LODs)为0.2~4.0 μg/kg, 定量限(limits of quantitative, LOQs)为0.6~10.0 μg/kg; 对于固体饮料, 方法检出限为1.0~20.0 μg/kg, 定量限为3.0~50.0 μg/kg。采用该方法对39例市售饮料样品进行分析, 3例碳酸饮料样品中检出香豆素, 含量为27.9~35.8 μg/kg, 测定值均低于现行方法标准中香豆素类化合物 50.0 μg/kg的测定低限。结论 该方法灵敏度高、定量限低, 且操作简便、快捷, 可满足同时测定饮料中8种香豆素类化合物含量的检测要求。

英文摘要:

      Objective To establish an analysis method for simultaneous determination of 8 kinds of coumarins in beverage by high performance liquid chromatography-tandem mass spectrometry. Methods The extraction effects of 8 kinds of coumarins from liquid beverage and solid beverage were investigated under different experimental conditions. Acetonitrile was used as extraction solvent, after the ultrasonic extraction and frozen centrifugation, and then the analytes were separated with C18 chromatographic column using 0.2% formic acid water and acetonitrile as mobile phase for gradient elution. Finally, the eluents were determined by multiple reaction monitoring (MRM) of electrospray ionization in positive mode, quantified by the matrix-matched external standard method. Results Good linearities in the range of 1?200 μg/L were observed for 8 kinds of target compounds, and the linear correlation coefficient (r2) were 0.9976?0.9999. The limits of detection (LODs) and limits of quantitative (LOQs) were 0.2?4.0 μg/kg and 0.6?10.0 μg/kg for liquid beverage, 1.0?20.0 μg/kg and 3.0?50.0 μg/kg for solid beverage, respectively. In this study, 39 commercial beverage samples were analysed using this method, and coumarin was detected in 3 carbonated beverage samples, the content range from 27.9 to 35.8 μg/kg. All measured values were lower than the LOQs of 50.0 μg/kg coumarin in the current method standard. Conclusion This method not only has high sensitivity and low LOQs, but also is simple, rapid, can meet the requirements of simultaneous determination of 8 kinds of coumarins in beverage.