Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection
Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection
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伯仲胺作为分散固相萃取净化中的吸附剂材料，用于通过电子捕获检测气相色谱法测定环境水样中的指示剂多氯联苯
DOI：
10.1002/jssc.201700315
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发表时间：
2017-08-01
影响因子：
3.1
通讯作者：
Jin, Yanjian
中科院分区：
文献类型：
--
作者：
Guo, Yuanming;Hu, Hongmei;Jin, Yanjian
建立了一种简便、快速、灵敏的气相色谱-电子捕获检测器（GC-ECD）测定水样中7种多氯联苯（PCBs）的新方法。首先用自动Jipad-6XB垂直振荡器使用正己烷/二氯甲烷（1：1，v/v）对含有30 g无水硫酸钠的1 L水样进行液-液萃取。用100 mg伯仲胺作为吸附剂材料，通过分散固相萃取净化浓缩的萃取物。该方法的线性范围为1.25 - 100 μ g/L，回归系数为0.9994 - 0.9999。检测限为纳克/升，范围为0.2至0.3纳克/升。自来水、湖水和海水中7种多氯联苯的外标回收率分别为85-112、76-116和72- 108%，相对标准偏差分别为3.3-4.5、3.4-5.6和3.1-4.8%（n = 5）。将该方法与传统的液-液萃取和固相萃取净化方法进行了比较，获得了相当的净化效率。该方法可用于不同水样中多氯联苯的测定。
A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1: 1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 mu g/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed methodwas compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples.