超声提取辅助浸入式固相微萃取-气相色谱/质谱技术快速检测土壤中的有机氯农药残留  

Rapid detection of organochlorine pesticide residues in soil by ultrasonic extraction-SPME-GC /MS technique

作　　者：曹国社 赖瑢[1] 周红 梁敏怡 卢城炜 欧阳钢锋[1] 朱芳[1] 

机构地区：[1]环境与能源广东省高校重点实验室,广东省环境污染控制与修复技术重点实验室,中山大学化学与化学工程学院,广州510275

出　　处：《环境化学》2014年第4期676-683,共8页Environmental Chemistry

基　　金：国家自然科学基金(21077137;21077135);广东省环境污染控制与修复技术重点实验室开放研究基金(2013k0009)资助

摘　　要：建立了超声提取辅助浸入式固相微萃取-气相色谱/质谱(DI-SPME-GC/MS)方法快速检测土壤中有机氯农残的新方法.该方法可实现分离、富集和进样一体化,减少样品前处理步骤.实验优化了DI-SPME的萃取条件、超声提取条件及GC/MS仪器参数.在优化条件下,9种OCPs在实验浓度范围(20—500 ng·g-1)内,线性关系良好,R2为0.9899—0.9987,方法检出限在0.67—1.76 ng·g-1,加标回收率在80.2%—117.1%,相对标准偏差(n=6)为10.0%—12.0%.结果表明该方法是一种简便快速、绿色环保的分析土壤中OCPs农残的方法.A new solid phase microextraction （SPME） method coulped with ultrasonic extraction and gas chromatography-mass spectrometry （GC/MS） technique was established for the rapid analysis of organochlorine pesticide （OCPs） residues in the soil was established. The method integrated isolation, enrichment and injection into one step and simplified the sample pretreatment procedure. In the experiment, the extraction conditions of SPME and ultrasonic extraction conditions as well as the GC/MS instrument parameters were optimized. Under the optimized conditions, calibration curves of 90CPs with good correlation coefficients （R2） from 0.9899 to 0.9987 were obtained. Limits of detection ranged from 0.67 ng· g-1 to 1.76 ng· g-1, and spiked recoveries ranging from 80.2% to 117.1% with relative standard deviations （RSDs,n= 6） of 10.0%-12.0% were observed. The results demonstrated that the developed method for the analysis of OCPs in soil samples was rapid, simple, and environmental friendly.

关 键 词：浸入式固相微萃取 超声提取 气相色谱-质谱 土壤 有机氯 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]