液相色谱-串联质谱法快速测定食品中的氟乙酸  

Rapid determination of fluoroacetic acid in food by liquid chromatography-tandem mass spectrometry

作　　者：张晶[1,2] 卢丽彬[1,2] 杨奕[1,2] 孟娟[1] 邵兵[1,2] 

机构地区：[1]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [2]首都医科大学公共卫生学院,北京100069

出　　处：《食品安全质量检测学报》2013年第3期660-664,共5页Journal of Food Safety and Quality

基　　金：国家科技支撑计划项目(2011BAK10B06);北京市卫生系统高层次卫生技术人才培养计划项目~~

摘　　要：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 develop a rapid method to detect fluoroacetic acid in foodstuffs by liquid chromatography tandem mass spectrometry(LC-MS/MS) and provide analytical methodology for the relevant food poison accidents.Methods Food samples were ultrasonically extracted with water,purified by a C18 cartridge,separated on a Waters ACQUITY UPLC CSH Fluoro-Phenyl column with gradient elution using acetonitrile and water containing 0.1% acetic acid at a flow rate of 0.3 mL/min and analyzed by liquid chromatography-tandem mass spectrometry.Mass data acquisition was conducted under the negative ion mode using multi-reaction monitoring.Results The method showed a good linearity over the range of 2.0~1000 μg/L for fluoroacetic acid with r2>0.99.Average recoveries of fluoroacetic acid fortified in soy sauce,vinegar,and cola samples at three spiked levels of 50,100,and 200 μg/kg were 82.4%~107.1% with relative standard deviations less than 20%.The detection limit(S/N≥3) and the limit of quantitation(S/N≥10) for the whole method were 10 μg/kg and 25 μg/kg,respectively.Conclusion Due to its simplicity,relatively high sensitivity and reproducibility,the method is suitable for the rapid detection of fluoroacetic acid in foodstuffs.It has been applied to analyze the target compound in the real food samples collected from two poisoning accidents.

关 键 词：液相色谱-串联质谱 食物中毒 毒物检测 氟乙酸 

分 类 号：R155.5[医药卫生—营养与食品卫生学]