漩涡辅助-分散液液微萃取-高效液相色谱法测定沉积物中的多环芳烃

引用本文: 冷庚, 吕桂宾, 陈勇, 尹辉, 但德忠. 漩涡辅助-分散液液微萃取-高效液相色谱法测定沉积物中的多环芳烃[J]. 分析化学, 2012, 40(11): 1752-1757. doi: 10.3724/SP.J.1096.2012.20398 shu

Citation: LENG Geng, LÜ Gui-Bin, CHEN Yong, YIN Hui, DAN De-Zhong. Determination of Polycyclic Aromatic Hydrocarbons in Sediment by High Performance Liquid Chromatography Following Vortex-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction[J]. Chinese Journal of Analytical Chemistry, 2012, 40(11): 1752-1757. doi: 10.3724/SP.J.1096.2012.20398 shu

漩涡辅助-分散液液微萃取-高效液相色谱法测定沉积物中的多环芳烃

冷庚 ^1, ,
吕桂宾 ^2, ,
陈勇 ^2, ,
尹辉 ^2, ,
但德忠 ^{1,
,}

通讯作者: 但德忠

摘要: 建立了漩涡辅助萃取(VAE)-分散液液微萃取(DLLME)-高效液相色谱法(HPLC)测定水系沉积物中多环芳烃(PAHs)的方法。对萃取剂和分散剂的种类及体积、萃取时间、盐效应及pH值等参数进行了优化。在优化条件下,方法检出限为2.3-6.8 ng/g,线性范围为10-2100 ng/g,相关系数0.9986-0.9994,低、中、高3个浓度水平的平均加标回收率分别为85.2%±4.7%, 85.0%±5.0%和85.0%±5.1%,平均相对标准偏差(RSD)分别为5.7%, 6.1%和5.7%。采用本方法对实际沉积物样品中PAHs进行分析,所有沉积物样品中均检出PAHs,3组不同采样深度沉积物样品中PAHs平均含量分别为73.3, 49.8和28.3 ng/g,平均加标回收率分别为84.8%±4.8%, 83.1%±4.7%和84.6%±4.6%。

关键词:

English

Determination of Polycyclic Aromatic Hydrocarbons in Sediment by High Performance Liquid Chromatography Following Vortex-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction

1.
¹ College of Architecture and Environment, Sichuan University, Chengdu 610065, China;

Corresponding author: 但德忠

Received Date: 16 April 2012

Abstract: A simple and rapid method, vortex-assisted extraction (VAE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction of polycyclic aromatic hydrocarbons (PAHs) in sediment samples prior to analysis by high performance liquid chromatography (HPLC)-fluorescence detection (FLD). Effects of significant parameters, such as type and volume of extraction and disperser solvent, extraction time, salt content and pH value, were optimized. Under the optimum conditions, the limits of detection (LODs) ranged from 2.3 to 6.8 ng/g, the linearity ranged from 10 to 2100 ng/g, coefficients of determinations (R²) ranged from 0.9986 to 0.9994. The average recoveries of PAHs in sediment samples spiking with 3 different concentration levels were 85.2%±4.7%, 85.0%±5.0% and 85.0%±5.1%, respectively, and the relative standard deviations were 5.7%, 6.1% and 5.7%, respectively. The proposed method was successfully applied in analysis of real nature sediment samples. PAHs were detected in all real nature sediment samples collecting from 3 different depths, the average amount in sediment samples were 73.3, 49.8 and 28.3 ng/g, respectively and the average recoveries was 84.8%±4.8%, 83.1%±4.7% and 84.6%±4.6%, respectively.

Key words:

Dispersive liquid-liquid microextraction
/ Vortex-assisted extraction
/ Polycyclic aromatic hydrocarbons
/ Sediment samples
/ High performance liquid chromatography-fluorescence detection

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通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

漩涡辅助-分散液液微萃取-高效液相色谱法测定沉积物中的多环芳烃

通讯作者: 但德忠

English

Determination of Polycyclic Aromatic Hydrocarbons in Sediment by High Performance Liquid Chromatography Following Vortex-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction

Corresponding author: 但德忠

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

漩涡辅助-分散液液微萃取-高效液相色谱法测定沉积物中的多环芳烃

通讯作者: 但德忠

English

Determination of Polycyclic Aromatic Hydrocarbons in Sediment by High Performance Liquid Chromatography Following Vortex-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction

Corresponding author: 但德忠

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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