液相色谱-串联质谱法快速测定食品中的氟乙酸
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, Waters ACQUITY 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 2.0~1000 μg/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、200 ug/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 10 ug/kg, 定量限为 25 ug/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 chro-matography 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.
标题：液相色谱-串联质谱法快速测定食品中的氟乙酸
英文标题：Rapid determination of fluoroacetic acid in food by liquid chromatography-tandem mass spectrometry
作者：
张晶 北京市疾病预防控制中心
卢丽彬 北京市疾病预防控制中心
杨奕 北京市疾病预防控制中心
孟娟 北京市疾病预防控制中心
邵兵 北京市疾病预防控制中心
中文关键词:液相色谱-串联质谱,食物中毒,毒物检测,氟乙酸,
英文关键词:liquid chromatography-tandem mass spectrometry,food poisoning,drug analysis,fluoroacetic acid,
发表日期：2013-06-08
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