气相色谱-串联质谱法测定土壤中十氯酮

研究了提取溶剂效率、净化方式等因素对十氯酮测定的影响,对比了加速溶剂提取、微波萃取及超声波等提取方式,考察了不同电子轰击能量、碰撞能量下特征离子对的响应。建立了加速溶剂萃取,H2SO4净化分离,气相色谱法-三重四极杆质谱法测定土壤中十氯酮的分析方法。取5.0 g土壤干样,内标法定量,线性相关系数为0.999 7,加标回收率为91.7%~121%,相对标准偏差为3.4%(n=6),检出限为0.1 ng/kg。

Determination of Chlordecone in Soil by Gas Chromatography-Tandem Mass Spectrometry

An analytical method to determine the concentration of Kepone in marine soil using gas chromatography-tandem mass spectrometry was developed. Several factors that may influence the analysis accuracy of Kepone in marine soil were investigated,such as extraction efficiency of different solvents and cleanup conditions. The efficiency of accelerated solvent extraction method,microwave extraction and ultrasonic extraction method was compared,and the effects of the response of the characteristics ion was investigated employing different energy electron bombardment and collision energies. The analytical method was developed by employing chromatography-tandem mass spectrometry under the condition of microwave extraction and cleanup with H₂SO₄. The dry soil samples (5.0 g) were extracted by the microwave extraction with the mixture of dichlormethane/acetone (1:1,V/V),the extracts were concentrated and cleaned up with H₂SO₄. Then the correlation coefficient was 0.9997,the average recoveries were between 91.7% and 121% with the relative standard deviation between 3.4% (n=6). The method detection limit was 0.1 ng/kg.