Optimization and validation of solid phase micro-extraction (SPME) method for analysis of polycyclic aromatic hydrocarbons in rainwater and stormwater
Optimization and validation of solid phase micro-extraction (SPME) method for analysis of polycyclic aromatic hydrocarbons in rainwater and stormwater
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DOI：
10.1016/j.pce.2009.07.003
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发表时间：
2009-01-01
影响因子：
3.7
通讯作者：
Balasubramanian, Rajasekhar
中科院分区：
文献类型：
--
作者：
Rianawati, Elisabeth;Balasubramanian, Rajasekhar
建立了一种简单、快速的固相微萃取(SPME) -气相色谱-质谱联用（GC-MS）法定量测定雨水和雨水样品中16种多环芳烃（PAHs）的方法。本研究优化了SPME法提取多环芳烃的条件，以达到水溶液中分析物的高富集。通过改变搅拌速率、盐浓度、纤维暴露时间、样品pH值和样品温度来优化该条件。结果表明，最佳提取工艺条件为：单氯乙酸钠浓度0.5 M，温度65℃，pH 7.0，搅拌720 rpm，提取时间60 min。15分钟的解吸时间可以消除残留。该方法具有良好的线性度、检出限和较高的富集系数，是一种灵敏的痕量水平测量工具。下一步，将新开发的SPME-GC-MS方法用于分析雨水和雨水样品中的多环芳烃，该方法在加尖合成雨水和雨水样品中具有较高的提取回收率。验证了该方法对实际雨水和雨水中多环芳烃的分析是可行的。爱思唯尔有限公司2009年版权所有版权所有。
This paper is about development of a simple and rapid solid-phase microextraction (SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) for the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAHs) in rainwater and stormwater samples. In this study the condition of PAHs extractions using SPME was optimized for achieving high enrichment of the analytes from aqueous samples. This condition was optimized by varying the stirring rate, salt concentration, fiber exposure time, sample pH, and sample temperature consecutively. The analysis revealed that optimal operating conditions occurred at condition of 0.5 M of sodium monochloroacetate, 65 degrees C, pH 7.0, agitation of 720 rpm, and an extraction time of 60 min. A desorption time of 15 min was shown to eliminate carry-over. The satisfactory linearity, detection limits and a high enrichment factor obtained prove that the method is a sensitive tool for trace level measurement. In the next step, the newly developed SPME-GC-MS method was validated for the analysis of PAHs in rainwater and stormwater samples, which resulted in high extraction recoveries from spiked synthetic rainwater and stormwater samples. This corroborates that the method is feasible for analysis of PAHs in real rainwater and stormwater analysis. Crown Copyright (C) 2009 Published by Elsevier Ltd. All rights reserved.