超声提取-气相色谱-质谱法快速测定配生土中16种多环芳烃化合物

Rapid determination of 16 polycyclic aromatic hydrocarbons in All-purpose Soil by ultrasonic extraction gas chromatography-mass Spectrometry

建立了一种快速测定配生土中16种多环芳烃化合物的超声提取-气相色谱-质谱方法。称取2.500 g配生土样品,于60℃超声波水浴中避光超声提取60 min,以4 000 r/min离心,移出上清液,残渣另用15 mL环己烷-丙酮(1∶1)超声提取30 min,重复提取2次,离心冷却后合并上清液。从上清液中准确移取10 mL,于30℃水浴,氮吹至约1 mL,溶液过硅酸镁净化小柱净化,过0.22μm尼龙有机针式滤膜,进样至气相色谱-质谱仪中测定。配生土中16种多环芳烃的检出限为0.01~0.02 mg/kg,16种多环芳烃样品加标回收率为71.2%~98.1%。该方法可快速测定绿化用配生土中16种多环芳烃化合物的含量。

A method for rapid determination of 16 polycyclic aromatic hydrocarbons(PAHs) in All-purpose Soil by ultrasonic extraction gas chromatography-mass spectrometry was established.2.500 g of the mixed soil sample was extracted in an ultrasonic water bath at 60 ℃ for 60 min,avoiding light,centrifugation was performed at 4 000 r/min to remove the supernatant.Repeated the ultrasonic extraction of the residue with 15 mL of cyclohexane and acetone(1:1) for 30 min.After centrifugation and cooling,merged the supernatant.Accurately 10 mL from the supernatant was transferred and blowed to about 1 mL in 30 ℃ water bath with nitrogen.The solution was purified by passing through a magnesium silicate purification column and passing through 0.22 μm nylon organic needle filter membrane,determined by gas chromatography-mass spectrometry.The detection limit of 16 kinds of polycyclic aromatic hydrocarbons in green planting soil was 0.01-0.02 mg/kg.Using this method,the spiked recovery experiment was carried out on raw soil samples,and the spiked recovery rate of 16 kinds of polycyclic aromatic hydrocarbons was 71.2%-98.1%.This method can quickly determine the content of 16 polycyclic aromatic hydrocarbons in All-purpose Soil.