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

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(3.143 s)为1.10~1.39μg·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8.06~233μg·kg^(-1),23.9~3148μg·kg^(-1),16.5~4106μg·kg^(-1)。

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(3.143 s)in the range of 1.10-1.39μg·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 8.06-233μg·kg^(-1) for DIBP,23.9-3148μg·kg^(-1) for DBP,and 16.5-4106μg·kg^(-1) for DEHP,respectively.