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

作　　者：侯德坤[1,2] 何江[1] 呼日乐达瓦 张福金[3] 张昕欣[3] 张敏[1] 张婷瑜 姚一萍[3] 

机构地区：[1]内蒙古大学环境与资源学院,呼和浩特010021 [2]国家海产品质量监督检验中心,威海264210 [3]内蒙古农牧业科学院资源环境与检测技术研究所,呼和浩特010031

出　　处：《理化检验（化学分册）》2015年第8期1049-1056,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金(21163006);内蒙古科技支撑项目(20110506);内蒙古自治区科技计划项目(20120438);内蒙古科技创新基金(2011CXJJN01)

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0．3～2．8μg·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。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 DDSMS 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.

关 键 词：气相色谱-串联质谱法 加速溶剂萃取 有机氯农药 松针 

分 类 号：O657.63[理学—分析化学]