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目的采用超高压液相色谱-电喷雾串联四极杆质谱建立了酱油、醋和可乐中的氟乙酸的快速检测技术,为相关中毒事件的样本分析提供方法学依据。方法食品样本用水稀释后经C18固相萃取小柱净化,WatersACQUITY UPLC CSH Fluoro-Phenyl色谱柱分离,以0.1%乙酸水和乙腈溶液为流动相梯度洗脱,最后用液相色谱-串联四极杆质谱仪在负离子MRM模式下测定。结果目标化合物在2.0～1000μg/L范围内线性良好,相关系数r2大于0.99。以酱油、醋和可乐为加标基质,在50、100、200μg/kg三个加标水平下氟乙酸的平均回收率为82.4%～107.1%,相对标准偏差小于20%,方法的检出限为10μg/kg,定量限为25μg/kg。结论该方法操作快速简单、灵敏度和重现性较好,成功用于两起氟乙酸中毒事件的样品检测。
OBJECTIVE To establish a rapid detection technique of fluoroacetic acid in soy sauce, vinegar and cola by ultra-high performance liquid chromatography-electrospray tandem mass spectrometry (ESI-MS / MS), and provide a methodological basis for sample analysis of related poisoning events. Methods The food samples were diluted with water and purified by a C18 solid phase extraction cartridge. WatersACQUITY UPLC CSH Fluoro-Phenyl columns were used to separate the samples. The mobile phase was eluted with 0.1% acetic acid in water and acetonitrile, and finally with liquid chromatography-tandem quadrupole The mass spectrometer was measured in negative ion MRM mode. Results The target compounds showed a good linearity in the range of 2.0-1000 μg / L and the correlation coefficient r2 was greater than 0.99. The average recoveries of fluoroacetic acid were 82.4% -107.1% at three spiked levels of 50, 100 and 200 μg / kg, with the relative standard deviation of less than 20%. The detection limits of the method 10μg / kg, the limit of quantification was 25μg / kg. Conclusion The method is rapid, simple, sensitive and reproducible and has been successfully applied to the detection of two fluoroacetic acidosis cases.