气相色谱/质谱法检测灰尘、土壤和沉积物中有机磷酸酯  

Analysis of Organophosphate Esters in Dust,Soil and Sediment Samples Using Gas Chromatography Coupled with Mass Spectrometry

作　　者：鹿建霞[1] 季雯[1] 马盛韬[2] 于志强[2] 王昭[1] 李寒[1] 任国发[1] 傅家谟[1,2] 

机构地区：[1]上海大学环境与化学工程学院环境污染与健康研究所,上海200444 [2]中国科学院广州地球化学研究所有机地球化学国家重点实验室,广东省环境资源与保护重点实验室,广州510640

出　　处：《分析化学》2014年第6期859-865,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.21007037,41273121);国家重大科技专项子课题(No.2009ZX07528-002-04);上海市重点学科项目(No.S30109)共同资助~~

摘　　要：本研究对实验过程中可能存在的污染源进行了定性筛查,采用不同的质控措施以降低实验过程中的背景污染。在严格的质控措施下研究了不同净化方法对样品中有机磷酸酯（OPEs）的净化效果,建立了气相色谱/质谱联用（GC/MS）检测灰尘、土壤和沉积物中7种主要OPEs的分析方法。以正己烷-二氯甲烷（1∶1,V/V）混合溶剂超声提取灰尘样品,以正己烷-丙酮（1∶1,V/V）索氏抽提土壤和沉积物样品中的待测组分,灰尘样品经一步固相萃取柱净化,土壤和沉积物样品经两步串联固相萃取柱联合净化后采用气相色谱/质谱进行定量。结果表明：采用上述净化手段,实验过程省时省力,基质去除率高,7种OPEs的回收率可稳定在67%以上。在高、低2个添加浓度水平下,不同基质样品（灰尘、土壤）中平均回收率为67.9%-117.4%;仪器检出限（LOD）为2.5-25.8μg/L,方法定量限（LOQ）分别为1.4-15.7 ng/g（灰尘）和0.3-2.9 ng/g（土壤）。采用此方法检测6份实际样品（包括2份灰尘样品、2份土壤样品、2份沉积物样品）,OPEs在所有样品中均有检出,其浓度范围分别在1313-1988 ng/g、29.9-32.0 ng/g和682-739 ng/g之间。Background contamination is a major problem in the analysis of organophosphate esters（ OPEs）. In this study,the possible sources of OPEs pollution were screened and several different ways were applied to minimize the blank contamination. Under the strict quality control measures,the cleanup efficiency of different solid phase extraction（ SPE） was investigated for OPEs in different environmental matrices. A method was developed for the detection of 7 OPEs in dust,soil and sediment samples by gas chromatograph coupled with mass spectrometry（ GC / MS）. Target compounds were extracted by hexane： dichloromethane（ 1∶ 1,V / V） followed by aminopropyl silica gel SPE column cleanup for dust,and target compounds in soil and sediment were Soxhlet extracted and cleanuped by two-step SPE. The results showed that the aminopropyl silica gel SPE column displayed the best purification performance among the three employed columns. Instrumental detection limits among the 7 OPEs ranged from 2. 5 to 25. 8 μg / L,and the method limits of quantification（ MLOQs） in dust and soil sample ranged from 1. 4 to 15. 7 ng / g and 0. 3 to 2. 9 ng / g,respectively. The average recoveries of 7 OPEs in different matrices（ dust and soil） at two spiked concentration levels ranged from 67. 9% to 117. 4%. The proposed method was successfully applied to detect OPEs in different environmental matrices collected in Shanghai.

关 键 词：有机磷阻燃剂 有机磷酸酯 气相色谱/质谱 土壤 沉积物 灰尘 

分 类 号：X830[环境科学与工程—环境工程] O657.63[理学—分析化学]