SPME-GCMS技术快速测定生态纺织品中持久性有机污染物(POPs).docVIP

SPME-GC/MS技术快速测定生态纺织品中持久性有机污染物（POPs） 蔡锦安1 刘丽琴2 阮文红1 朱芳1* (1 中山大学化学与化学工程学院， 广州 510275；2 广州市纤维产品检验院， 广州 510220) 摘 要: 建立了固相微萃取-气相色谱/质谱法（SPME-GC/MS）快速同时测定生态纺织品中10种持久性有机污染物(POPs)的方法。探讨了影响SPME萃取效果的萃取纤维、萃取时间和温度、萃取液离子强度和pH、脱附时间等因素，并对生态纺织品中持久性有机污染物(POPs)的提取液配方进行了优化。实验结果表明，最佳萃取条件为：100μm PDMS萃取纤维头、萃取时间25min、萃取温度为室温、脱附时间4min、萃取液盐含量2%NaCl以及pH值为6.0。该方法检测10种POPs的线性范围宽，校正曲线的相关系数在0.9906-0.9988之间，方法重现性好，RSD值在3.2%-13.2%之间，检测限均低于30μg/L。对实际样品（100%棉织物）进行加标回收实验，回收率在70.0%-112.6%之间。 关键词：持久性有机污染物(POPs)；固相微萃取（SPME）；生态纺织品；气相色谱-质谱联用 Application of solid-phase microextraction for the determination of persistent organic pollutants in textiles by gas chromatography with mass spectrometry Jin’an Cai1, Liqin Liu2, Wenhong Ruan1, Fang Zhu1* (1 School of Chemistry and Chemical Engineering, Sun Yat-sun University, Guangzhou 510275, China; 2 Guangzhou Institute of Textiles Fibres Analysis, Guangzhou 510220, China) Abstract: A method based on solid-phase microextraction (SPME) and gas chromatography with mass spectrometry (GC/MS) for the determination of ten persist organic pollutants (POPs) in ecological textiles sample was described. Commercially available SPME fibers, 100 μm PDMS, 85 μm PA, 75 μm PDMS-DVB, 75 μm CAR/PDMS and 30 μm PDMS were compared and 100 μm PDMS exhibited better performance to the POPs. The parameters affecting SPME procedure, including extraction and desorption time, extraction temperature, salinity and pH, were studied. The optimized conditions were 25 min extraction at room temperature, 5 % NaSO4 content, pH 6.0, and 4.0 min desorption in GC injector port at 250 °C. The linear ranges of the SPME-GC/MS method were 0.1-500 μg/L for. Dieldrin and Endrin, 1.0-500 μg/L for Hexachlorobenzene(HCB)，16-500 μg/L for cis-Chlordane and trans-Chlordane, 20-500 μg/L for o,p-DDT, p,p-DDT, 40-500 μg/L for Heptachlor, Aldrin and Mirex. The limits of detection ranged from 0.04μg/L (Dieldrin) to 29.62 μg/L (Aldrin) and the RSDs were between 3.2% and 13.3%. The optimized method was then used to