加速溶剂萃取凝胶渗透色谱联合固相萃取净化-气相色谱质谱法测定土壤中的6种多环麝香  

Determination of 6 Polycyclic Musks in Soil by ASE-GPC-SPE Purification and GC-MS Detection

作　　者：罗庆[1] 王诗雨 孙丽娜[1] 王辉[1] 

机构地区：[1]沈阳大学区域污染环境生态修复教育部重点实验室,辽宁沈阳110044

出　　处：《沈阳大学学报（自然科学版）》2017年第5期362-366,373,共6页Journal of Shenyang University：Natural Science

基　　金：国家重点基础研究发展规划资助项目(2014CB441100);国家科技重大专项基金资助项目(2012ZX07202004)

摘　　要：通过对萃取、净化和检测等条件的优化,建立了土壤中萨利麝香、粉檀麝香、特拉斯麝香、开许梅龙、佳乐麝香和吐纳麝香等6种多环麝香的加速溶剂萃取-凝胶渗透色谱与固相萃取协同净化-气相色谱质谱检测方法.采用V(正己烷)∶V(丙酮)=1∶1的混合溶剂作为萃取溶剂,在100℃下静态萃取5min,并循环2次;萃取液浓缩后进入凝胶渗透色谱系统,采用V(环己烷)∶V(乙酸乙酯)=1∶1的混合溶剂作为流动相进行洗脱,收集7.5~15.0min的洗脱液;洗脱液浓缩后进入已用10mL正己烷活化的硅胶填料的固相萃取小柱,采用10mL二氯甲烷洗脱,收集洗脱液并浓缩定容;采用气相色谱质谱联用技术在选择离子扫描模式下进行检测.该方法6种多环麝香的加标回收率为81.3%~106.6%,相对标准偏差为6.4%~11.5%,方法检出限为0.56~0.72μg·kg^(-1),方法定量限为1.88~2.39μg·kg^(-1).A new method using ASE combined with GPC and SPE cleanup followed by GC-MS detection has been established for the quantitative determination of six polycyclic musks in soil.In the method,the samples were extracted by ASE with V（hexane）∶V（acetone）=1∶1 at 100℃for 5 min,and cycle 2 times.After evaporated to dryness,the extract was dissolved in 10 mL V（cyclohexane）∶V（ethyl acetate）=1∶1 and injected into GPC column with V（cyclohexane）∶V（ethyl acetate）=1∶1 as the mobile phase at a flow rate of 4.7 mL·min（-1）.The 7.5-15.0 min fraction was collected for subsequent analysis.The portions collected from GPC were dissolved in 1 mL hexane after evaporated to dryness.Then the 1 mL extractions were purified by SPE using silica gel column,eluted with 10 mL dichloromethane.Finally,the eluate was dissolved in 1 mL hexane after evaporated to dryness,and then analyzed by GC-MS in the Selective Ion Monitor（SIM）mode.The correlation coefficient of each polycyclic musk was r20.99,the average recoveries were in the range of 81.3%-106.6%.The RSD ranged from 6.4% to 11.5%.The method detection limit（MDL）is 0.56-0.72μg·kg（-1）,and the method quantitative limit（MQL）is 1.88-2.39μg·kg（-1）.

关 键 词：多环麝香 加速溶剂萃取 固相萃取 凝胶渗透色谱 气相色谱质谱联用 

分 类 号：X833[环境科学与工程—环境工程]