流动注射-高分辨飞行时间质谱检测毒饵大米中的氟乙酰胺
Detection of Fluoroacetamide in Rice Bait Using Hydrolysis-Flow Injection by HR-TOF-MS
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摘要: 采用氨水加热水解氟乙酰胺 -流动注射 -大气压电喷雾电离 -高分辨飞行时间质谱检测氟乙酰胺水解产物氟乙酸负离子。该方法具有离子质量检测误差小 (误差 <1 m D)、专属性强、简便快速、灵敏度高等特点 ,可检测氟乙酰胺含量为 1 0 μg/g的毒饵大米 ,大米空白不产生干扰。讨论了针对氟乙酸负离子检测的仪器参数优化、负离子质量校正物选择、内标选择、氟乙酰胺水解条件和水解率、检测方法的精密度等。对该方法在其它样品的应用前景做了推测。Abstract: The raticide fluoroacetamide (FAA) is detected by HR-TOF-MS using flow injection (FI). The FAA is first hydrolyzed with 10% amonia in boiling water bath to produce fluoroacetic acid, and fluoroacetic acid as the hydrolysis product is detected. The mass deviation is less than 1 mD (77.004 5 vs 77.003 9) with 5-sulfosalicyic acid as calibration mass. The only possible mass interference within ±10 mD is C 2H 6OS which can be identified by its M+2 peak abundance. 10 μg/g FAA in rice bait can be detected. The parameters of TOF-MS are discussed. There is no interference in blank rice. The whole procedure from sample preparation to FI-TOFMS detection can be finished within 1 h.