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    加速溶剂萃取-气相色谱-串联质谱法测定松针中16种有机氯农药残留方法的中心组合设计优化

    Optimization of GC-MS/MS Determination of Residual Amounts of 16 Organochlorine Pesticides in Pine Needle with Accelerated Solvent Extraction Based on Design-Expert

    • 摘要: 采用加速溶剂萃取-气相色谱-串联质谱法测定松针中16种有机氯农药的残留量,并对萃取条件进行了优化.在气相色谱分离中用DB-5MS石英毛细管柱为固定相,在质谱分析中采用总离子扫描监测模式.16种有机氯农药在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.3~2.8 μg·L-1之间.方法用于松针样品分析,加标回收率在80.9%~99.2%之间,测定值的相对标准偏差(n=7)在2.9%~8.4%之间.

       

      Abstract: GC-MS/MS was applied to the determination of residual amounts of 16 organochlorine pesticides in pine needle with accelerated solvent extraction.Extraction conditions of accelerated solvent extraction were optimized.The DB-5MS quartz capillary chromatographic column was used for GC separation and the total ion current monitoring mode were adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 16 organochlorine pesticides were kept in definite ranges.Detection limits (3S/N) found were ranged from 0.3 to 2.8 μg·L-1.The proposed method was applied to the analysis of samples of pine needle,giving values of recovery and RSD′s (n=7) in the ranges of 80.9%-99.2% and 2.9%-8.4%,respectively.

       

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