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目的建立大米中59种有机磷、有机氯、氨基甲酸酯、拟除虫菊酯四类农药残留量的免净化气相色谱串联质谱(GC-MS/MS)简便快速的测定方法。方法样品经打碎、过筛,用5m L正己烷振荡提取,低温离心,取上清液用GCMS/MS直接进样检测。结果本法59种农药在2.00μg/kg~100μg/kg范围内呈良好线性关系,相关系数r>0.995;检出限(LOD)0.001μg/kg~3.5μg/kg,定量下限(LOQ)0.004μg/kg~12μg/kg,相对标准偏差0%~17.7%(n=6),回收率80.0%-108%。结论本法简便、快速、灵敏、准确,适用于大米中59种农药残留的检测。
Objective To establish a simple and rapid method for the determination of four kinds of pesticide residues in rice by GC-MS / MS, including 59 kinds of organophosphorus, organochlorine, carbamate and pyrethroid. Methods The samples were disrupted, sieved, extracted with 5 mL of n-hexane, centrifuged at low temperature, and supernatants were directly injected by GCMS / MS. Results The results showed that there was a good linear relationship between 59 pesticides in the range of 2.00μg / kg ~ 100μg / kg and the correlation coefficient r> 0.995. The limit of detection (LOD) was 0.001μg / kg ~ 3.5μg / kg, μg / kg ~ 12μg / kg. The relative standard deviations were 0% ~ 17.7% (n = 6). The recoveries were 80.0% -108%. Conclusion This method is simple, rapid, sensitive and accurate and suitable for the detection of 59 kinds of pesticide residues in rice.