Hu Hongmei, Guo Yuanming, Sun Xiumei, Chen Xuechang, Zhang Xiaoning, Liu Qin, Xu Chunxiu
1Zhejiang Province Key Lab of Mariculture & Enhancement, Marine Fishery Institute of Zhejiang Province, Zhoushan 316100, China.
J Chromatogr Sci. 2014 May-Jun;52(5):375-82. doi: 10.1093/chromsci/bmt043. Epub 2013 May 3.
A simple, rapid, sensitive and high throughput method is described, based on solid-phase disk extraction (SPDE) and gas chromatography-electron capture detection, for the determination of chlorobenzens (CBs) in water samples. The proposed SPDE sample pretreatment method was initially optimized and the optimum experimental conditions were found to be as follows: 500 mL water sample (pH 2.5) extracted and enriched by an Empore 3-stn C18 (octadecyl) SPE disk at flow rate of 5 to 50 mL/min, eluted by 5 mL of acetone and 3 × 5 mL of methylene dichloride. The linearity of the method ranged from 0.02 to 0.4 µg/L for dichlorobenzene isomers, 0.0022-0.044 µg/L for trichlorobenzene isomers, 0.005-0.01 µg/L for tetrachlorobenzene isomers and 0.00025 to 0.005 µg/L for pentachlorobenzenes and hexachlorobenzenes, with correlation coefficients ranging between 0.9991 and 0.9999. The limits of detection were in the low ng/L level, ranging between 0.05 and 4 ng/L. The recoveries of spiked CBs with the external calibration method at different concentration levels in deionized/distilled water, tap water and sea water samples were 99-115, 91-106% and 96-110%, respectively, and with relative standard deviations of 4.5-7.6, 4.2-6.8 and 3.6-6.6% (n = 5), respectively. It is concluded that this method can successfully be applied for the determination of CBs in deionized/distilled water, tap water and sea water samples.
本文描述了一种基于固相圆盘萃取(SPDE)和气相色谱 - 电子捕获检测的简单、快速、灵敏且高通量的方法,用于测定水样中的氯苯(CBs)。所提出的SPDE样品预处理方法首先进行了优化,发现最佳实验条件如下:500 mL水样(pH 2.5)以5至50 mL/min的流速通过Empore 3 - stn C18(十八烷基)固相萃取盘进行萃取和富集,用5 mL丙酮和3×5 mL二氯甲烷洗脱。该方法的线性范围为:二氯苯异构体为0.02至0.4 μg/L,三氯苯异构体为0.0022 - 0.044 μg/L,四氯苯异构体为0.005 - 0.01 μg/L,五氯苯和六氯苯为0.00025至0.005 μg/L,相关系数在0.9991至0.9999之间。检测限处于低ng/L水平,范围为0.05至4 ng/L。在去离子水/蒸馏水、自来水和海水样品中,采用外标法在不同浓度水平加标CBs的回收率分别为99 - 115%、91 - 106%和96 - 110%,相对标准偏差分别为4.5 - 7.6%、4.2 - 6.8%和3.6 - 6.6%(n = 5)。结论是该方法可成功应用于测定去离子水/蒸馏水、自来水和海水样品中的CBs。