摘要
应用液液萃取、固相萃取柱、固相萃取盘等传统和现代富集技术,对半挥发性有机物进行提取,建立了气相色谱-负化学电离质谱测定地下水中毒杀芬的方法。对性能较好的自制GDX-502固相萃取柱进行了条件优化。结果表明,使用填制的GDX-502固相萃取柱富集地下水中的毒杀芬,基体加标回收率为92.3%～98.5%,优于商品固相苯取柱LC-C18、ENVITM-C18以及固相萃取盘(92.8%～96.8%)和液液萃取(80.3%～88.5%);GDX-502固相萃取柱富集速度低于固相萃取盘,但远高于LC-C18和ENVITM-C18;GDX-502固相萃取柱的批量处理样品能力(12个)高于固相萃取盘(6个);同时所使用的有机试剂量远低于液液萃取。GDX-502固相萃取柱的萃取效率、分析通量、经济性和环保性具有更大的优势。
Toxaphene is a broad-spectrum organochlorine insecticide, which was one of the most widely used pesticides worldwide. It was listed as an organic contaminant in the Stockholm Convention on Persistent Organic Pollutants （2001） and the Groundwater Pollution Survey Specification of the China Geological Survey （2006）, respectively, because of persistence and adverse effects on humans and the ecosystem. In this study, three methods of extraction of toxaphene from ground water samples were compared using liquid-liquid extraction, a solid phase extraction cartridge and solid phase extraction disc. The analytical conditions were optimized detailed for GDX-502 solid phase extraction （SPE） cartridge lab-filled because of its excellent character. The research results show that GDX-502 SPE cartridge packed in the lab has the highest recoveries （92.3% -98.5% ） in three SPE cartridges such as GDX-502, commercial LC-C18 and ENVITM-C18, and is also better than a solid phase extraction disc （92.8% -96.8% ） ＆ liquid-liquid extraction （80.3% -88.5% ）. The extraction time of the SPE disc only needs 20 -30 min for single extraction, and less than 40 -50 rain of GDX-502 SPE cartridge, 200 rain of LC-C18 and ENVITM-C18. The GDX-502 SPE processes 12 samples as a batch which is more than 6 for the SPE disc. The SPE disc has the highest analytical cost and the GDX-502 SPE is cheaper than the SPE disc. The SPE is considered environmentally friendly because its solvent amounts are less than those for liquid-liquid extraction. Finally, the GDX-502 solid-phase extraction cartridge has more advantages in terms of extraction efficiency, throughput, cost and environmental protection.
出处
《岩矿测试》
CAS
CSCD
北大核心
2012年第4期653-659,共7页
Rock and Mineral Analysis
基金
中国地质大调查项目(1212011120283
1212010816028)
国土资源部公益性行业科研专项(200911043-28)
关键词
地下水
毒杀芬
液液萃取
固相萃取柱
固相萃取盘
气相色谱-负化学电离质谱法
under groundwater
toxaphene
liquid-liquid extraction
soli phase extraction cartridge
solid phaseextraction disc
Gas Chromatography-Negative Ion Chemical Ionization-Mass Spectrometric
