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

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

Determination of tetrabromobisphenol-A in electronic waste area soil by gas chromatography-mass spectrometry

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^-1The repeatability （RSD） equals 2.52%. The response obtained withthis method was linear over the range assayed, 20-400 μg·kg^-1ith 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^-1est result of TBBPA from electronic waste in the surrounding agriculture soil area 0.312-4.170 μg·kg^-1