气相色谱-三重四级杆串联质谱法测定湖泊沉积物中的有机氯农药  

Determination of Organochlorine Pesticides Residues in Lake Sediment by Using Gas Chromatography-( Tandem) Mass Spectrometry

作　　者：李超灿[1,2] 霍守亮[2] 席北斗[2] 

机构地区：[1]沈阳航空航天大学,辽宁沈阳110136 [2]中国环境科学研究院,北京100012

出　　处：《环境工程技术学报》2013年第5期422-428,共7页Journal of Environmental Engineering Technology

基　　金：国家水体污染控制与治理科技重大专项(2009ZX07106-001);国家自然科学基金项目(40901248)

摘　　要：建立了索氏提取、气相色谱-三重四级杆串联质谱（GC-MS/MS）分析湖泊沉积物中20种有机氯农药的方法。样品萃取液经硅胶氧化铝层析柱净化,使用不同配比二氯甲烷、正己烷混合溶剂对吸附在层析柱上的目标物进行洗脱,洗脱液浓缩后进GC-MS/MS检测。应用三重四级杆串联质谱仪的多级反应监测模式,配以有机氯农残分析专用VF-1701色谱柱,完全排除了沉积物基质干扰,对目标化合物进行精准的定性定量分析,简化了前处理过程。该方法灵敏度较高,仪器的线性范围良好。基质样品加标回收率为79.76%~115.04%,相对标准偏差为1.15%~14.08%。方法检出限为0.002 4~0.513 7μg/kg,方法定量限为0.007~1.541μg/kg。该方法适合检测沉积物中痕量有机氯农药残留。A sohxlet-extraction-gas chromatography-（tandem） mass spectrometry（GC-MS/MS） as a tool for 20 organochlorine pesticides residue analysis in lake sediment was developed.Chromatographic column of silica gel and alumina was employed to remove impurities in the concentrated extraction by different ratios of hexane and dichloromethane eluents.Then the concentrated eluent was analyzed by the gas chromatography-（tandem） mass spectrometry.The matrix interferences were eliminated owing to Multiple Reaction Monitoring（MRM） mode of GCMS/MS together with the Chromatographic column of VF-1071.The pretreatment was simplified and accurately qualitative and quantitative analysis of the target compounds was supplied.This method was of high sensitivity and showed a good linearity.Recoveries obtained by analyzing the spiked standard in matrix were in the range of 79.76%-115.04%,whereas the relative standard deviation（RSD） values were ranging from 1.15% to 14.08%.The method detection limit was between 0.002 4 and 0.513 7 μg/kg and limits of quantification of the method were between 0.007 and 1.541 μg/kg.This new method is stable and reliable for trace analysis of organochlorine pesticides residues in the sediment.

关 键 词：气相色谱-三重四级杆串联质谱 有机氯农药 沉积物 

分 类 号：X830.2[环境科学与工程—环境工程]