基质固相分散辅助加速溶剂萃取-气相色谱-质谱法测定道路扬尘中9种邻苯二甲酸酯的含量
Determination of 9 Phthalic Acid Esters in Road Dust by Gas Chromatography-Mass Spectrometry with Matrix Solid Phase Dispersion Assisted Accelerated Solvent Extraction
安彩秀 1赫彦涛 1刘淑红 1李然 1史会卿 1杨利娟1
作者信息
- 1. 河北省地质实验测试中心,保定 071051;河北省矿产资源与生态环境重点实验室,保定 071051
- 折叠
摘要
道路扬尘样品成分复杂且没有相应的标准检测方法,基于将加速溶剂萃取(ASE)与基质固相分散(MSPD)相结合,提出了题示方法.取 10.0 g道路扬尘样品与 10.0 g弗罗里硅土搅拌均匀,装入萃取池(预先加入一层厚度约 0.5 cm的硅藻土),用体积比 1∶1的正己烷-二氯甲烷混合液于100℃萃取 2 次.将萃取液浓缩至 5.0 mL左右,氮吹至 1.0 mL左右,用正己烷定容至 1.0 mL,采用气相色谱-质谱法测定其中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPRP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸苄基丁基酯(BBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸(2-乙基己基)酯(DEHP)和邻苯二甲酸正辛酯(DNOP)等 9 种邻苯二甲酸酯(PAEs)的含量.结果表明,9 种PAEs 标准曲线的线性范围均为0.1～5.0 mg·L-1,检出限(3.143s)为 1.10～1.39 μg·kg-1.按照标准加入法进行回收试验,回收率为 76.6%～107%,测定值的相对标准偏差(n=6)小于 10%.方法用于实际样品分析,DIBP、DBP和DEHP的检出量较高,依次为 8.06～233 μg·kg-1,23.9～3 148 μg·kg-1,16.5～4 106 μg·kg-1.
Abstract
The composition of road dust samples was complex and there was no corresponding standard detection method.Based on this fact,a method mentioned by the title was proposed by combining accelerated solvent extraction(ASE)with matrix solid phase dispersion(MSPD).The road dust sample(10.0 g)was mixed well with 10.0 g of floritic silica,then put into the extraction tank(pre-adding a layer of diatomaceous earth with a thickness of about 0.5 cm),and extracted twice with a mixture of n-hexane-dichloromethane at a volume ratio of 1∶1 at 100℃.The extract was concentrated to about 5.0 mL,and then blown to about 1.0 mL by nitrogen.Its volume was made up to 1.0 mL with n-hexane,in which 9 phthalic acid esters(PAEs),including dimethyl phthalate(DMP),diethyl phthalate(DEP),dipropyl phthalate(DPRP),diisobutyl phthalate(DIBP),dibutyl phthalate(DBP),benzyl butyl phthalate(BBP),dicyclohexyl phthalate(DCHP),phthalate(2-ethylhexyl)ester(DEHP),and n-octyl phthalate(DNOP),were determined by gas chromatography-mass spectrometry.As shown by the results,the linear range of the standard curves of 9 PAEs was 0.1-5.0 mg·L-1,with detection limits(3.143s)in the range of 1.10-1.39 μg·kg-1.Test for recovery was made by the standard addition method,giving results in the range of 76.6%-107%,with RSDs(n=6)of the determined values less than 10%.This method was applied to analysis of the actual samples,with higher detection amounts of 8.06-233 μg·kg-1 for DIBP,23.9-3 148 μg·kg-1 for DBP,and 16.5-4 106 μg·kg-1 for DEHP,respectively.
关键词
邻苯二甲酸酯/加速溶剂萃取/基质固相分散/气相色谱-质谱法/道路扬尘Key words
phthalic acid ester/accelerated solvent extraction/matrix solid phase dispersion/gas chromatography-mass spectrometry/road dust引用本文复制引用
基金项目
河北省地矿局地质科技项目(454-0601-YBN-DONH)
保定市科技支撑计划(2011ZF011)
河北省地矿局地质科技项目(454-0502-JBN-BBNP)
出版年
2024
NETL
NSTL
万方数据