超声萃取-高效液相色谱法测定土壤中苯并[a]芘研究

采用超声萃取-高效液相色谱荧光检测法对土壤中苯并a]芘含量进行定性、定量分析.土壤样品用正己烷/二氯甲烷(1+1)超声萃取,萃取液经硅胶柱或佛罗里硅土柱净化浓缩定容,乙腈-水为流动相,线性梯度洗脱,流速为1.0 mL/min,荧光检测器激发波长为280 nm,发射波长为420 nm,外标法峰面积定量.结果显示:该方法检出限低,苯并a]芘的检出限为0.15μg/kg.这种方法具有很好的精密度,相对标准偏差为3.9%~8.4%.实际水样加标回收率范围在72.5%~85.8%.能够满足土壤的监测要求.

Determination of Benzo(a) -pyrene in Soil by Ultrasound Extraction and High Performance Liquid Chromatography

A novel method for detection and determination ofbenzo( a) -pyrenein soil was developed, using ultrasound ex-traction-HPLC. Soil samples were extracted with hexane/dichloromethane(1+1)ultrasonic extraction, extract by silica gel col-umn or Florisil silica column purification for volume and concentration, acetonitrile water as mobile phase, linear gradient elution, a flow rate of 1. 0 ml/min, fluorescence detector excitation wavelength was at 280 nm and emission wavelength of 420 nm, exter-nal standard method and peak area quantification. . Result showed that the limit of detection for benzo( a) -pyrene was0. 15μg/kg. The method can accurately determine benzo( a) -pyrene, the relative standard deviation was in the range of 3. 9% ~8. 4%. The real sample results showed that the recovery ratio of standard addition was in the range of 72. 5% ~85. 8%. Therefore the method can well satisfy the need of practical determination in soil.