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    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

    • 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.

       

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