【摘要】 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。更多还原

【Abstract】 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-1with 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。更多还原