CAJ | 학술논문

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。
본연구건립기상색보/질보래측정전자랄급탁해구토양중사추쌍분 A（TBBPA）적방법。해화합물통과초성파보조췌취，용제선택V(병동）﹕V(정기완）=1﹕1혹을산을지；정화주선택산화적불라리규토화무수류산납혼합물혹CleanertC18-SPE진행정화；정화액농축후경연생반응，연생시제선용N,O-쌍（삼갑기규완기）삼불을선알（BSTFA）화함1%적삼갑기록규완（TMCS）。해방법측정전자랄급탁해구토양중TBBPA적검출한위(S/N=3)0.1μg·kg-1，가표회수솔평균치위92.7%（n=5），중현성RSD위2.52%(n=5)；선성범위시20～400μg·kg-1，상관계수0.999。해방법용우조사전자랄급탁해구토양중사추쌍분A，범위치위5.17～218.00μg·kg-1；기주위농전토양중사추쌍분A，범위치위0.312～4.170μg·kg-1。
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.