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目的应用分析保护剂补偿基质效应,建立气相色谱-串联质谱(GC-MS/MS)测定水果中27种有机磷农药的方法。方法样品经乙腈提取,Qu ECh ERS净化,引入分析保护剂(古洛糖酸内酯和D-山梨醇),采用GC-MS/MS,多重反应监测(MRM)的扫描方式测定,外标法定量。结果添加分析保护剂后,27种有机磷农药的浓度为0.10μg/ml~4.00μg/ml时,线性相关系数得到很好的改善,线性相关系数均>0.995,方法的检出限为0.003 mg/kg~0.013 mg/kg,方法的定量限为0.010 mg/kg~0.043 mg/kg,加标回收率为75.7%~115%,相对标准偏差(RSD)为2.4%~8.7%。结论本方法采用Qu ECh ERS前处理方法,大大简化了前处理步骤,引入分析保护剂能显著补偿由基质增强效应造成的定量误差,具有较高的选择性和灵敏度,适合水果中27种有机磷农药的检测。
OBJECTIVE: To analyze the effect of substrate for compensatory effects of protective agents and establish a method for the determination of 27 organophosphorus pesticides in fruits by gas chromatography-tandem mass spectrometry (GC-MS / MS). Methods The samples were extracted with acetonitrile and cleaned up with Qu ECh ERS. The protective agents (gulonolactone and D-sorbitol) were introduced and analyzed by GC-MS / MS and multiplex reaction monitoring (MRM) Quantitative. Results When the concentration of 27 organophosphorus pesticides was 0.10μg / ml ~ 4.00μg / ml, the linear correlation coefficient was improved after the protective agent was added. The linear correlation coefficients were both> 0.995. The detection limit was 0.003 mg / kg ~ 0.013 mg / kg. The limit of quantification was 0.010 mg / kg ~ 0.043 mg / kg. The recoveries were 75.7% ~ 115%. The relative standard deviations (RSDs) ranged from 2.4% to 8.7%. Conclusion The method of Qu ECh ERS pretreatment greatly simplifies the pretreatment steps. The introduction of the protective agent can significantly compensate the quantitative error caused by the matrix enhancement effect, and has high selectivity and sensitivity. It is suitable for the determination of 27 kinds of organic phosphorus Pesticide testing.