中华医学超声杂志

应用化学 ›› 2011, Vol. 28 ›› Issue (11): 1298-1304.DOI: 10.3724/SP.J.1095.2011.00729

• 研究论文 • 上一篇    下一篇

α-环糊精修饰有机聚合物整体材料选择性富集室温磷光法测定土壤中的萘

张雪,龚晓娜,朱若华*   

  1. (首都师范大学化学系 北京 100048)
  • 收稿日期:2010-12-09 修回日期:2011-01-30 出版日期:2011-11-10 发布日期:2011-11-10
  • 通讯作者: 朱若华，教授; Tel:010-68903047; Fax:010-68903047; E-mail:zhurh@mail.cnu.edu.cn; 研究方向：发光分析
  • 基金资助:
    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）

Determination of Naphthlene in Soil Samples by Room Temperature Phosphorescence with Selective Enrichment on α-Cyclodextrin Modified Monolithic Material

ZHANG Xue, GONG Xiaona, ZHU Ruohua*   

  1. (Department of Chemistry，Capital Normal University，Beijing 100048)
  • Received:2010-12-09 Revised:2011-01-30 Published:2011-11-10 Online:2011-11-10
  • Contact: ZHU

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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。

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

Abstract:

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.

Key words: Organic polymeric monolithic substrate, α-cyclodextrin, solid phase extraction, room temperature phosphorescence, polycyclic aromatic hydrocarbon

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