优化QuEChERS结合HPLC测定沉积物中14种多环芳烃  

Determination of 14 Polycyclic Aromatic Hydrocarbons in Sediment by HPLC Coupled with Optimized QuEChERS

作　　者：吕爱娟[1] 沈小明[1] 时磊[1] 蔡小虎[1] 沈加林[1] 胡璟珂[1] 

机构地区：[1]中国地质调查局南京地质调查中心,江苏南京210016

出　　处：《中国环境监测》2017年第1期115-120,共6页Environmental Monitoring in China

基　　金：地质大调查项目"持久性有机污染物实验技术与分析方法研究"(1212011120274)

摘　　要：以美国国家标准技术研究院(NIST)2种沉积物标样SRM 1944和SRM 1941b为研究对象,建立并优化了QuEChERS结合HPLC测定沉积物中14种多环芳烃的前处理方法,并与传统索氏提取进行比较。优化后的QuEChERS方法:样品经乙腈浸泡后,超声15 min,漩涡振荡3 min,以NaCl和无水MgSO_4盐析,提取液经PSA净化后经HPLC-FLD测定。该条件下14种PAHs的方法检出限为0.5~5.0μg/kg,SRM 1944和SRM 1941b中PAHs回收率分别为73.4%~104.9%和71.9%~96.4%,相对标准偏差分别为0.47%~3.45%和0.87%~3.05%。索氏提取SRM 1944与1941b回收率分别为78.9%~109.3%和80.9%~108.2%,相对标准偏差分别为1.46%~10.3%和1.27%~10.8%。优化后的QuEChERS回收率与索氏提取较为接近,但具有更高的精密度。将该方法用于实际海洋沉积物提取,PAHs测定值与索氏提取较为接近。优化后的QuEChERS方法满足批量沉积物样品中PAHs的快速测定要求。The preparation method for determination of 14 polycyclic aromatic hydrocarbons （ PAHs） in sediment using reference materials SRM1944 and SRM1941b from the National Institute of Standards and Technology （NIST） by high performance liquid chromatographic （ HPLC） coupled with modified QuEChERS was developed, and compared with Soxhlet extraction. Route for the optimized QuEChERS method was： Samples soaked with acetonitrile, ultrasonic extracted 15 minutes, vortex oscillated 3 minutes, and were salted out by NaCl and MgSO4 , then the extraction solvent was cleaned up with PSA, analyzed by HPLC with fluorescence detector. The limits of detection for 14 PAHs under optimum conditions were in the range of 0.5.5.0 μg/kg. Recovery rates for PAHs by QuEChERS and Soxhlet extraction in SRM1944 and SRM1941b were ranged from 73.4%-104.9%, 71.9%-96.4% and 78.9%-109.3%, 80.9%-108.2%, with relative standard deviations 0.47%-3.45%, 0.87%-3.05% and 1.46%-10.3%, 1.27%-10.8%. Recovery rates of optimized QuEChERS were in agreement with Soxhlet extraction, but with higher precision. This method was applied in the determination of PAHs in marine sediment, and the results were close to Soxhlet extraction. The optimized QuEChERS method meets the requirement for the rapid determination of PAHs in batch sediment samples.

关 键 词：QuEChERS优化 多环芳烃 沉积物 高效液相色谱 

分 类 号：X833[环境科学与工程—环境工程]