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超声萃取-高效液相色谱法测定沉积物中多环芳烃 被引量:12

HPLC Determination of Polycyclic Aromatic Hydrocarbons in Sediment with Ultrasonic Extraction
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摘要 提出了高效液相色谱法测定沉积物中多环芳烃(PAH′s)含量的方法。样品中多环芳烃用正己烷-丙酮(1+1)混合溶液超声提取,离心分离后,所得萃取液经蒸发浓缩,然后过装有1g无水硫酸钠和2g硅胶的层析柱净化。以Varian PAHs色谱柱为分离柱,不同比例配成的甲醇和水为流动相梯度洗脱,用荧光检测器检测。方法的检出限(3S/N)在0.34~1.52ng.g-1之间。方法用于沉积物中多环芳烃的测定,测定结果的相对标准偏差(n=5)在3.2%~10.6%之间。用标准加入法测定方法的回收率,结果在57.1%~103. Contents of polycyclic aromatic hydrocarbons(PAH′s) in sediment were determined by HPLC.The PAH′s in the sample were extracted ultrasonically with a mixture of n-hexane-acetone(1+1).After centrifugation,the extract was evaporated,concentrated and purified with chromatographic column packed with 1 g of Na2SO4 and 2 g of silica gel.Varian PAHs chromatographic column was used as stationary phase,and solutions of methanol mixed with water in different ratios were used as mobile phase in the gradient elution.The eluate from the column was used for HPLC analysis with fluorescence detector.Detection limits(3S/N) of the method found were in the range of 0.34-1.52 ng·g-1.The proposed method was used in determination of PAH′s in sediment,giving values of RSD′s(n=5) in the range of 3.2%-10.6%.Recovery found by standard addition method were in the range of 57.1%-103.4%.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2012年第3期308-311,共4页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金 河南省重点科技攻关项目(No.072102350025) 河南省教育厅自然科学基础研究计划(2009A610007)
关键词 超声萃取 高效液相色谱法 荧光检测器 多环芳烃 沉积物 Ultrasonic extraction HPLC Fluorescent detector Polycyclic aromatic hydrocarbons Sediment
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