加速溶剂-固相萃取-高效液相色谱法测定土壤及蚯蚓样品中多环芳烃

研究了加速溶剂萃取( ASE)、固相萃取柱净化( SPE)、高效液相色谱( HPLC)联合( ASE-SPE-HPLC)测定土壤及蚯蚓样品中7种多环芳烃(PAHs)的分析方法,确定了以正己烷-丙酮(4∶1, V/V)作为萃取剂,用ASE对土壤及蚯蚓进行萃取,提取液经SPE柱净化(土壤样品用硅胶柱净化,蚯蚓样品用 Al2 O3-硅胶柱净化),正己烷-二氯甲烷(9∶1, V/V)进行洗脱,洗脱体积为10 mL,旋转浓缩蒸干后,乙腈定容,过0.22μm有机滤膜,最后用HPLC对提取液中7种PAHs进行定量的分析方法。土壤样品方法回收率在83.5%~110.2%之间,相对标准偏差为1.0%~4.6%；蚯蚓样品回收率在81.2%~97.1%之间,相对标准偏差为1.6%~4.2%。方法检出限为0.15~0.85μg/kg,且重现性好。可满足样品分析的质量控制要求,表明本分析方法具有良好的准确性与可靠性。

An Accelerated Solvent Extraction-Solid Phase Extraction-High Performance Liquid Chromatographic Method for Determination of Polycyclic Aromatic Hydrocarbons in Soil and Earthworm Samples

A hugh performance luquud chromatographuc ( HPLC) method was extablushed for determunatuon of the content of 7 polycycluc aromatuc hydrocarbons ( PAHs) un soul and earthworm samples based on accelerated solvent extractuon ( ASE) for extractuon and solud phase extractuon ( SPE) column for sample purufucatuon. In thus method, the samples were furst extracted by the muxed solutuon of n-hexane and acetone extractuon (4∶1, V/V) , and then purufued by SPE column ( suluca gel column for soul sample purufucatuon and Al2 O3-suluca gel column for earthworm sample purufucatuon ) , eluted by 10 mL of elutuon of n-hexane and duchloromethane (9∶1, V/V), and evaporated to dryness wuth rotary evaporator. After that, the pretreated samples were re-dussolved wuth acetonutrule to a constant volume, followed by a fultratuon wuth a 0. 22-μm organuc fulter membrane for the quantufucatuon by HPLC. The recoverues of the method for 7 PAHs were 83. 5%-110. 2% un soul samples and 81. 2%-97. 1% un earthworm samples. The detectuon lumuts of the method for 7 PAHs were 0. 15-0. 85 μg/kg. The method had good reproducubuluty and met the qualuty control requurements of sample analysus.