摘要
合成了α-环糊精(α-CD)修饰的有机聚合整体材料,对合成的材料进行了表征,研究比较了α-CD修饰整体材料作为室温磷光固体基质的效果以及14种有机化合物在其上的室温磷光分析(RTP)行为。α-CD修饰的有机聚合整体材料背景干扰低,对二环芳烃类物质有较好的选择性和富集能力。在α-CD修饰膜上,萘和7,8苯并喹啉的分配常数分别为5.03×103和2.94×102,表明修饰材料对萘有较好的选择性。萘酚也能与修饰材料形成包络物。但是由于较强的极性和在水中的溶解性,不能被有效富集。对5.0×10-11 mol/mL萘,最大富集体积为300 mL。采用SPE-RTP,萘和7,8苯并喹啉的检出限分别为9.80×10-12和4.60×10-11 mol/mL,RSD小于3.7%;线性范围分别为5.00×10-11～8.00×10-9 mol/mL和6.00×10-11～5.00×10-10 mol/mL。应用修饰的膜片对土样中的萘进行选择性富集和测定,结果由GC-MS进一步确认。用环己烷一步提取和SPE-RTP测定,萘可以被选择性富集。在土壤样品中加萘标准0.012 8 mg,测得回收率(104.9±6.5)%。土样中萘的浓度为(5.61±0.12)mg/kg,与GC-MS的较为吻合。
The α-cyclodextrin（CD） modified organic monolithic materials were synthesized and applied for the enrichment of polyaromatic compounds from environmental samples.Application of the modified materials in the solid extraction-room temperature phosphores（SPE-RTP） were studied and compared.The room temperature phosphorescence behaviors of 14 organic compounds on the α-CD modified substrate were examined.Compared with the β-CD modified material,the α-CD modified monolithic materials have less RTP background and therefore better sensitivity as well as enrichment capabilities for the double ring aromatic substances.The partition constants of naphthlene and 7,8-benzoquinolin on α-CD modified monolith were found to be 5.03×103 and 2.94×102,respectively,indicating that α-CD modified monolith has higher selectivity for naphthlene.Naphthol can form inclusion complex also with α-CD modified monolith.However,because of the large polarity and solubility in water,the extraction efficiency at higher concentration is relatively low.The largest enrichment volume for the concentration of 5×10-11 mol/mL naphthlene is 300 mL.With SPE-RTP,the detection limits for naphthlene and 7,8-benzoquinolin are 9.80×10-12 mol/mL and 4.60×10-11 mol/mL,respectively.The linear ranges are 5.00×10-11~8.00×10-9 mol/mL and 6.00×10-11 ~5.00×10-10 mol/mL,respectively,with RSD less than 3.7%.α-CD modified membrane was applied to the determination of naphthalene in polluted soil samples and results were further verified by GC-MS.With one step extraction by cyclohexane and then followed by SPE-RTP,naphthlene can be selectively concentrated from soil samples.With 0.012 8 mg naphthlene spiked in the soil samples,the recovery is（104.9±6.5）%.The concentration of naphthlene in the soil samples was determined as（5.61±0.12） mg/kg,which was in accord with the results of GC-MS.
出处
《应用化学》
CAS
CSCD
北大核心
2011年第11期1298-1304,共7页
Chinese Journal of Applied Chemistry
基金
国家自然科学基金(20875065)资助项目
北京市属市管高校人才强教计划知识创新团队(PHR20100718)
关键词
有机聚合整体材料
Α-环糊精
固相萃取
室温磷光
多环芳烃
organic polymeric monolithic substrate
α-cyclodextrin
solid phase extraction
room temperature phosphorescence
polycyclic aromatic hydrocarbon
