摘要
利用点击反应对含叠氮基的溶胶-凝胶整体柱进行了表面修饰，制备了 C6-硅胶杂化整体萃取柱。实验以多环芳烃为分析对象，考察了制备和修饰条件对萃取效率的影响，在优化的条件下，新制备的整体柱对萘、菲、芘和苯并[a]芘的萃取富集倍数分别达到95.9、114.2、103.2和57.8。萃取实验的日内和日间精密度（RSD）分别小于5.5％（ n=8）和7.3％（ n=10）。建立的管内固相微萃取-高效液相色谱检测16种常见多环芳烃方法的检出限（ S／N=3）达到0.08~3.72μg／L，定量限（ S／N=10）达到0.26~12.40μg／L。土壤中多环芳烃分析的加标回收率为82.4％~110.6％，RSD为2.6％~7.9％（ n=3）。与美国国家环境保护局检测土壤中多环芳烃的方法比较，结果一致，准确性高。实验表明，该方法萃取效率高，灵敏可靠，操作简便，重现性好，可满足土壤等样品中痕量多环芳烃检测的要求。
A C6-silica hybrid monolithic column was prepared by click reaction with capillary sil-ica monolith. Firstly,an azide-functionalized silica monolithic column was synthesized via sol-gel reaction with tetramethoxysilane（TMOS）and 3-azidopropyltrimethoxysilane（N3PTMS）. Then 1-hexyne was covalently immobilized on the capillary monolith by the“azide-alkyne”click reaction to form C6-silica hybrid monolithic column. As an extraction media of polycyclic aromatic hydro-carbons（ PAHs）,the conditions for the preparation and modification of the monolith were care-fully investigated according to the extraction efficiency. The enrichment factors for typical PAHs：naphthalene,phenanthrene,pyrene and benzo[a]pyrene finally reached 95. 9,114. 2,103. 2 and 57. 8,respectively. The relative standard deviations（ RSDs）for the extraction were lower than 5. 5%（ intra-day,n=8）and 7. 3%（ inter-day,n=10）. Based on the in-tube solid phase microex-traction（ in-tube SPME）,a new determination method for 16 PAHs was developed with high per-formance liquid chromatography（ HPLC）. The limits of detection（ LODs,S/N=3）were 0. 08-3. 72 μg/L and the limits of quantification（ LOQs,S/N=10）were 0. 26-12. 40μg/L for the PAHs. The spiked recoveries for the PAHs in soil samples were between 82. 4% and 110. 6% with the RSDs（ n=3）of 2. 6%-7. 9%. Comparison with the method of United States Environmental Protec-tion Agency（U. S. EPA）for the PAHs determination in soil samples,the results showed good accuracy and high consistency. And the high extraction efficiency with high sensitivity and con-venience was also demonstrated in the applications of the new approach.
出处
《色谱》
CAS
CSCD
北大核心
2015年第5期455-460,共6页
Chinese Journal of Chromatography
基金
河南省科技发展计划项目(122102310333,1223041346)
河南省教育厅基础前沿项目(13A150793)
关键词
点击反应
硅胶杂化整体柱
管内固相微萃取
高效液相色谱
多环芳烃
click reaction
silica hybrid monolith
in-tube solid phase microextraction （SPME）
high performance liquid chronmtography （HPLC）
polycyclic aromatic hydrocarbons （PAHs）
