首页> 中文期刊> 《生态环境学报》 >气相色谱/质谱测定电子垃圾拆解区土壤中四溴双酚A的方法

气相色谱/质谱测定电子垃圾拆解区土壤中四溴双酚A的方法

         

摘要

The determination of derivatized tetrabromobisphenol-A in soil sample from electronic waste area by gas chromatography-massspectrometry was developed in this study. The compounds wereextracted from soil by sonication assisted extractionin small columns (SAESC) with a low Volume of the mixture of acetone and hexane (V: V= 1:1) or ethylacetate as extraction solvent.; an acidified Florisil-anhydrous sodium sulfate mixture or CleanertC18-SPE was carried out to remove interferences; N, O-bis(trimethylsilyl) trifluoroacetamide(BSTFA) and 1% trimethyl chlorosilane was used as derivating agent. Average recoveries from spiked samples were 92.7%(n=5) and the estimated limits of detection (S/N=3) varied 0.1 µg·kg-1. The repeatability (RSD) equals 2.52%. The response obtained withthis method was linear over the range assayed, 20-400 µg·kg-1 with correlation coefficients equalor higher than 0.999. The validated method was used to investigate the levels of TBBP-A compounds in soil samples in electronic wastearea, Testresult 5.17-218.00 µg·kg-1;Test result of TBBPA from electronic waste in the surrounding agriculture soil area 0.312-4.170 µg·kg-1.%本研究建立气相色谱/质谱来测定电子垃圾拆解区土壤中四溴双酚 A(TBBPA)的方法。该化合物通过超声波辅助萃取,溶剂选择V(丙酮)﹕V(正己烷)=1﹕1或乙酸乙酯;净化柱选择酸化的氟罗里硅土和无水硫酸钠混合物或CleanertC18-SPE进行净化;净化液浓缩后经衍生反应,衍生试剂选用N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)和含1%的三甲基氯硅烷(TMCS)。该方法测定电子垃圾拆解区土壤中TBBPA的检出限为(S/N=3)0.1µg·kg-1,加标回收率平均值为92.7%(n=5),重现性RSD为2.52%(n=5);线性范围是20~400µg·kg-1,相关系数0.999。该方法用于调查电子垃圾拆解区土壤中四溴双酚A,范围值为5.17~218.00µg·kg-1;其周围农田土壤中四溴双酚A,范围值为0.312~4.170µg·kg-1。

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