Determination of phthalate esters in soil by low pressure headspace solid phase microextraction-gas chromatography-tandem mass spectrometry
Zhejiang Institute of Metrology, Hangzhou 310018, China
PDMS/DVB-65 μm固相微萃取纤维，加入1 mL盐溶液， 0.1kPa的顶空压力和80℃的萃取温度作为最佳实验条件，采用气相色谱-串联质谱法进行测定，外标法定量。6种酞酸酯类化合物的含量在5～800 μg/kg范围内与色谱峰面积具有良好的线性关系，相关系数均不小于0.992，检出限为0.5～4.2 μg/kg，定量限为1.7～14 μg/kg。样品加标回收率为79.4％～102.8%，测定结果的相对标准偏差为7.5％～14.1%(n =5)。采用该方法和加速溶剂萃取法对实际土壤进行检测，结果表明，该方法对实际土壤中DMP，DEP，DBP，BBP，DEHP和DNOP 6种酞酸酯类化合物均具有较好的提取富集效果。该方法为土壤环境中酞酸酯类有机污染物的测定提供了更环保的技术手段。
Abstract：A method for the determination of phthalate esters in soil by low pressure headspace solid phase micro extraction-gas chromatography-tandem mass spectrometry was established. PDMS/DVB-65 μm solid phase microextraction fiber, the volume of 1 mL salt solution, 0.1 kPa headspace pressure and 80℃ extraction temperature were selected as the optimal experimental conditions. Gas chromatography-tandem mass spectrometry was used for determination, and external standard method was used for quantitative analysis. The content of the 6 phthalate esters had a good linear relationship with the chromatographic peak area in the range of 5-800 μg/kg, the correlation coefficients were not less than 0.992, the detection limits were 0.5-4.2 μg/kg, and the limits of quantification were 1.7-14 μg/kg. The recoveries were 79.4%-102.8%, and the relative standard deviations of determination results were 7.5%-14.1%(n =5). The method and accelerated solvent extraction method were used to detect the actual soil. The results showed that the method had good extraction and enrichment effect of DMP, DEP, DBP, BBP, DEHP and DNOP in actual soil samples. The method provides a more environmentally friendly approach for the determination of phthalate organic pollutants in soil.
Keywords：low pressure; solid phase microextraction; phthalate esters; gas chromatography-tandem mass spectrometry; soil
HE H. Determination of phthalate esters in soil by low pressure headspace solid phase microextraction-gas chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage，2020，29(6)：83-88.