快速溶剂萃取-气相色谱-三重四极杆质谱法测定沉积物中的酞酸酯  

Determination of phthalate esters in sediment by accelerated solvent extraction and gas chromatography-triple quadrupole mass spectrometry

作　　者：罗财红[1] 郭志顺[1] 孙静[1] 

机构地区：[1]重庆市环境监测中心,重庆401147

出　　处：《色谱》2010年第5期487-490,共4页Chinese Journal of Chromatography

基　　金：国家"863"计划项目(No.2007AA061602)

摘　　要：建立了快速溶剂萃取(ASE)-气相色谱-三重四极杆质谱(GC-MS/MS)测定沉积物中酞酸酯的方法。样品用二氯甲烷-丙酮(体积比为1∶1)混合溶剂在100℃、103.4MPa(1500psi)条件下经快速溶剂萃取、以5mL/min的速率经凝胶渗透色谱(GPC)净化去除大分子干扰物后,采用GC-MS/MS分析测定。采用内标法定量,17种酞酸酯的检出限为0.05～0.40μg/kg;回收率为50.5%～107.9%,相对标准偏差为3.5%～13.9%。采用替代物基体加入法对方法的性能进行了验证,3种替代物的回收率为65.3%～95.8%。该方法快速、灵敏度高,能同时准确定性定量测定17种酞酸酯。A method for the determination of seventeen phthalate esters in sediment by accelerated solvent extraction （ASE）,gel-permeation chromatography （GPC） and gas chromatography-triple quadrupole mass spectrometry （GC-MS/MS） has been developed. The target compounds were extracted at 100 ℃ and 103.4 MPa （1 500 psi） by ASE using the mixtures of dichloromethane and acetone （1∶1,v/v） as solvent. In order to eliminate the interferences from larger molecular sizes,the extract was purified at a flow rate of 5.0 mL/min by GPC. Following that,the extract was concentrated to a final volume of 1 mL exactly. The GC-MS/MS was applied to quantitative and qualitative analysis. Internal standard calibration approach was adopted,and the detection limits of seventeen phthalate esters ranging from 0.05 to 0.40 μg/kg were obtained. The correlation coefficients were beyond 0.996,the recoveries were from 50.5% to 107.9%,and the relative standard deviations were from 3.5% to 13.9%. Besides,the surrogate compounds spiked were used to monitor the performance of the method,and the recoveries were from 65.3% to 95.8% for the three surrogate compounds. The method is fast,sensitive and exact for analyzing seventeen phthalate esters simultaneously.

关 键 词：快速溶剂萃取 气相色谱-三重四极杆质谱 酞酸酯 沉积物 

分 类 号：O658[理学—分析化学]