引用本文:翟有朋,顾云,丁金美.高效液相色谱法测定土壤中多环芳烃的条件优化[J].环境监控与预警,2018,10(1):17-21
ZHAI You peng, GU Yun, DING Jin mei.Optimization of Conditions for Determination of PAHs in Soil by HPLC[J].Environmental Monitoring and Forewarning,2018,10(1):17-21
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高效液相色谱法测定土壤中多环芳烃的条件优化
翟有朋,顾云,丁金美
泰州市环境监测中心站,江苏 泰州 225300
摘要:
研究了加速溶剂萃取(ASE)、固相萃取柱净化(SPE)、高效液相色谱仪(HPLC)联合测定土壤中16种多环芳烃(PAHs)的分析方法,选择以正己烷/丙酮(1+1,V/V)作为ASE提取溶剂,提取液经SPE硅胶小柱净化,正己烷/二氯甲烷(1+1,V/V)进行洗脱,洗脱体积为10 mL,洗脱液经旋转蒸发浓缩至近干,过0.22 μm有机滤膜,用乙腈定容至1 mL,最后用 HPLC-紫外检测器对提取液中16种PAHs进行定量分析。土壤中16种PAHs的方法检出限为2.8~4.9 μg/kg,加标回收率为81.9%~102%,相对标准偏差为2.5%~6.2%,完全满足土壤中PAHs分析的质量控制要求,该法稳定性好、准确度高、可操作性强,适合于土壤样品中16种PAHs 的准确测定。
关键词:  加速溶剂萃取  固相萃取  高效液相色谱  土壤  多环芳烃
DOI:
分类号:X833:O657.72+
文献标识码:B
基金项目:
Optimization of Conditions for Determination of PAHs in Soil by HPLC
ZHAI Youpeng, GU Yun, DING Jinmei
Taizhou Environmental Monitoring Center, Taizhou,Jiangsu 225300,China
Abstract:
The analysis method of 16 kinds of PAHs in soil was studied by accelerated solvent extraction, solid phase extraction purification and high performance liquid chromatograph. nHexane/acetone (1+1,V/V) was selected as ASE solvent, the extracts were purified by silica column,nhexane/dichloromethane (1+1,V/V) was used as elution solvent, the elution volume was 10 mL.The elution solution was concentrated to nearly dry by rotary evaporation, and then was filtered by 0.22 μm organic membrane, finally acetonitrile was added to make up to the 1 mL mark.Quantitative analysis were taken by HPLC equipped with UV detector. The method detection limits were 2.8~4.9 μg/kg, the average spiked recoveries were 81.9%~102%,the relative standard deviations were 2.5%~6.2%, which completely satisfy the requirement for quality control of PAHs analysis in soil.This method had good stability, high accuracy and strong practicality, it was suitable for accurate determination of 16 kinds of PAHs in soil samples.
Key words:  Accelerated solvent extraction  Solid phase extraction  High performance liquid chromatograph  Soil  PAHs