固相微萃取/气相色谱-质谱联用技术在有机磷酸三酯阻燃剂土壤吸附分析中的应用  

SPME/GC-MS for Studying Adsorption of Organophosphate Flame Retardants on Soils

作　　者：郑春莉[1] 冯珊珊[1] 杜苗苗[1] 齐月[1] Elke FRIES 

机构地区：[1]西安交通大学环境工程系,西安710049 [2]Federal Institute for Geosciences and Natural Resources,im Geozentrum Hannover

出　　处：《西安交通大学学报》2015年第11期128-134,共7页Journal of Xi'an Jiaotong University

基　　金：国家自然科学基金资助项目(21307097);陕西省工业攻关资助项目(2014K10-02);中央高校基本科研业务费专项资金资助项目(2012jdhz39)

摘　　要：以3种常用且极性相差较大的有机磷酸三酯阻燃剂(OPFRs)作为研究对象,采用固相微萃取/气相色谱-质谱(SPME/GC-MS)联用技术建立了一种适用于研究OPFRs土壤吸附的分析方法:优化固相微萃取的萃取条件——取样体积为7mL,萃取时间为30min,解吸温度和时间分别为270℃和5min;分析测定过程中导致空白值升高的干扰因素;针对不同类型的土壤分别绘制标准曲线。利用已建立的SPME/GC-MS法对3种OPFRs在不同类型土壤中的吸附程度进行了初步评估,结果表明:3种OPFRs在试验土壤中的吸附率为27%~69%,吸附程度随着OPFRs极性的减弱以及土壤有机质含量的增加而增加。该方法具有操作简单,分析速度快,准确度、灵敏度和精密度均能满足定量测试要求,空白干扰小以及易于普及等特点。Three kinds of commonly used organophosphate flame retardants （OPFRs） with different polarities were selected as the research object in this study. Solid phase microextraction coupled with gas chromatography-mass spectrometry （SPME/GC-MS） was adopted to develop an analytical method to study the adsorption performance of OPFRs in soils. The SPME conditions, such as extraction time, sampling volume, desorption time and desorption temperature, were optimized. The interference factors leading to the increase of blank values were determined. Different calibration curves of OPFRs were established for each tested soil sample. Based on the SPME/GC-MS method, the adsorption performance of three OPFRs in different soils was preliminarily investigated. The results showed that the adsorption rate of three OPFRs in the tested soils ranged from 27^-69~, and the adsorption rate increased with the decrease in OPFRs＇ polarity and the increase in the organic matter content in the tested soils. The analytical method developed in this study is easy to operate with quick speed, high accuracy and sensitivity for quantitative test of OPFRs. In addition, this method has little blank interference, and is easy to be popularized.

关 键 词：固相微萃取 有机磷酸三酯阻燃剂 土壤 吸附 

分 类 号：O641[理学—物理化学] O647[理学—化学]