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目的建立气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)同时检测乙酰甲胺磷和甲胺磷的残留量。方法通过正交试验优化并确定升温程序参数,利用液液萃取方法从水中提取乙酰甲胺磷及甲胺磷后,采用基质匹配标准溶液对两种农药的回收率进行校准。结果升温程序应采用一阶程序升温,初始温度为95℃,升温速度为10℃/min,末温为280℃;进样口采用惰性衬管;添加水平为0.1~1 mg/L时,回收率在80.3%~110.5%之间,相对标准偏差在5.5%~6.5%之间。乙酰甲胺磷和甲胺磷在用纯溶剂(丙酮)和空白基质配制0.01~0.5 mg/L浓度范围内线性关系良好(r~2>0.999),乙酰甲胺磷和甲胺磷的检出限分别为0.02mg/L、0.008 mg/L,定量检测分别为0.066 mg/L、0.027 mg/L。结论该方法的精密性、重复性和稳定性良好,可适用于乙酰甲胺磷和甲胺磷残留量的检测。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) for simultaneous determination of acephate and methamidophos residues. Methods Orthogonal test was used to optimize and determine the parameters of the temperature program. After the extraction of acephate and methamidophos from water by liquid-liquid extraction, the recoveries of the two pesticides were calibrated using matrix matching standard solution. Results The temperature program should be programmed by the first-order procedure with an initial temperature of 95 ° C, a heating rate of 10 ° C / min and a final temperature of 280 ° C. An inert liner was used for the inlet and was withdrawn at 0.1-1 mg / L Rates ranged from 80.3% to 110.5% with relative standard deviations between 5.5% and 6.5%. Acephate and methamidophos showed good linearity (r ~ 2> 0.999) in the range of 0.01-0.5 mg / L with pure solvent (acetone) and blank matrix. The detection of acephate and methamidophos The limits of detection were 0.02mg / L and 0.008 mg / L respectively, and the quantitative detection was 0.066 mg / L and 0.027 mg / L, respectively. Conclusion The method has good precision, repeatability and stability and is suitable for the determination of acephate and methamidophos residues.