论文部分内容阅读
目的建立一种自动选择离子扫描-气相色谱-质谱联用法(Auto Sim-GC-MS)同时测定蔬菜、水果中多种农药残留的方法。方法样品匀浆后,用乙腈提取,经Carb/NH2柱净化,最后氮吹浓缩。样品处理液经气相色谱毛细管柱分离后,质谱仪采用全扫描及自动选择离子扫描方式进行分析,对目标物进行定型,外标法定量。结果该方法可同时对36种农药准确定性、定量分析;在50 ng/ml~400 ng/ml时,各组分的标准曲线相关系数均>0.99,线性关系良好,满足分析要求。方法的回收率为82.5%~115.0%,平均相对标准偏差(RSD)为3.42%~8.98%,检出限为0.005 mg/kg~0.010 mg/kg。结论该方法简便、灵敏,精密度和准确度均能满足实验要求,特别是自动选择离子扫描模式比传统扫描模式更加快速、简便,适用于大批量蔬菜、水果中多种农药残留的快速分析。
Objective To establish a method for the simultaneous determination of multiple pesticide residues in vegetables and fruits by automatic selective ion-scan-gas chromatography-mass spectrometry (Auto Sim-GC-MS). Methods After the sample was homogenized, it was extracted with acetonitrile, purified by a Carb / NH2 column, and finally concentrated by nitrogen. After the sample solution was separated by gas chromatography capillary column, the mass spectrometer was analyzed by full scan and automatic selection of ion scan mode, and the target was shaped and quantified by external standard method. Results The method could accurately and quantitatively analyze 36 kinds of pesticides at the same time. The correlation coefficients of the standard curves of all the components were> 0.99 at 50 ng / ml ~ 400 ng / ml, and the linear relationship was good and satisfied the analytical requirements. The recoveries were 82.5% ~ 115.0%. The average relative standard deviations (RSDs) were 3.42% ~ 8.98%. The limits of detection were 0.005 mg / kg ~ 0.010 mg / kg. Conclusion The method is simple, sensitive, precise and accurate to meet the experimental requirements. In particular, the auto-selected ion scan mode is faster and easier than the traditional scanning mode and is suitable for the rapid analysis of a large number of pesticide residues in vegetables and fruits.