Application of silica-based monolith as solid-phase extraction sorbent for extracting toxaphene congeners in soil
Application of silica-based monolith as solid-phase extraction sorbent for extracting toxaphene congeners in soil
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DOI：
10.1007/s10971-016-4054-8
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发表时间：
2016-10-01
影响因子：
2.5
通讯作者：
Chen, Yongsheng
中科院分区：
文献类型：
--
作者：
Ma, Xiaodong;Zhao, Mengying;Chen, Yongsheng
开发了一种硅胶整体柱作为固相萃取吸附剂，用于从土壤提取液中提取和分离毒杀芬同系物，然后通过气相色谱-质谱法对其进行测量。采用扫描电子显微镜、透射电子显微镜、N2吸附/脱附和傅里叶变换红外光谱对硅胶整体柱进行了表征。对洗脱剂种类、洗脱剂体积、流速和吸附剂用量等回收参数进行了系统优化。方法的检出限较低，六氯、七氯、八氯和九氯毒杀芬的检出限分别为1.64、0.76、1.03和2.28 ng/mL。该吸附剂在200-1000 ng/mL浓度范围内线性关系良好，相关系数r（2）> 0.99。毒杀芬同系物的相对回收率在96.8 - 105.7%之间，相对标准偏差（% RSD）小于5%。该吸附剂连续使用5次后，毒杀芬的回收率为99.9%~ 104.0%，表明该吸附剂具有良好的稳定性和可重复使用性。
A silica monolith was developed as a solid-phase extraction sorbent for the extraction and separation of toxaphene congeners from soil extraction solutions, prior to their measurement by gas chromatography-mass spectroscopy. The silica monolith was characterized by scanning electron microscopy, transmission electron microscopy, N-2 adsorption/desorption and Fourier transform infrared spectroscopy. The recovery parameters including type of eluent, eluent volume, flow rate and varying amounts of sorbent were systemically optimized. Our method has a low detection limit, and it was 1.64, 0.76, 1.03 and 2.28 ng/mL for hexachloro, heptachloro, octachloro and nonachloro toxaphene, respectively. The sorbent offered good linearity with coefficient of determination (r (2)) > 0.99, over a concentration range of 200-1000 ng/mL. The relative recoveries of toxaphene congeners ranged between 96.8 and 105.7 % with relative standard deviations (% RSD) below 5 %. The recoveries of toxaphene congeners were 99.9-104.0 % after using the sorbent five times, showing the excellent stability and reusability of prepared silica monolith sorbent.