Huang Zhoubing, Liu Shuqin, Xu Jiangqiao, Yin Li, Sun Fen, Zhou Ningbo, Ouyang Gangfeng
College of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Yueyang 414006, PR China.
MOE Key Laboratory of Bioinorganic and Synthetic Chemistry, School of Chemistry, Sun Yat-Sen University, No. 135, Xingang Xi Road, Guangzhou, Guangdong 510275, PR China.
Talanta. 2018 Feb 1;178:629-635. doi: 10.1016/j.talanta.2017.09.090. Epub 2017 Oct 1.
The introduction of functional groups into metal organic frameworks has great potential for enhancement in adsorption performance of nitrosamines using solid phase microextraction (SPME). However, pre-functionalization and post-modification generally suffer from the same limitation that the additional functional groups occupy the free volume and thereby decreasing pore volume and special surface area. Herein, we use a modulator-induced defect-formation strategy to prepare the 8-aminocaprylic acid doped UIO-66 (Am-UIO-66) with high adsorption capacity of nitrosamines. Then, the as-synthesized UIO-66 and Am-UIO-66 were fabricated as SPME fibers exhibiting good adsorption capacity towards nitrosoamines. The reason was that the 8-aminocaprylic acid creates structural defects and additional pore spaces of Am-UIO-66, thus increases the specific surface area as well as pore volume. Finally, the Am-UIO-66-coated SPME fiber was successfully applied to the determination of nitrosamines migration from latex gloves and achieved good linearity (20-2000ngL), satisfactory recoveries (85.2-112.8%) and rather low LODs (2.61-6.12ngL), by coupling with gas chromatography-mass spectrometry (GC-MS).
将官能团引入金属有机骨架对于利用固相微萃取（SPME）提高亚硝胺的吸附性能具有巨大潜力。然而，预官能化和后修饰通常存在相同的局限性，即额外的官能团占据了自由体积，从而降低了孔体积和比表面积。在此，我们采用调节剂诱导缺陷形成策略制备了具有高亚硝胺吸附能力的8-氨基辛酸掺杂的UIO-66（Am-UIO-66）。然后，将合成的UIO-66和Am-UIO-66制成对亚硝胺具有良好吸附能力的SPME纤维。原因是8-氨基辛酸造成了Am-UIO-66的结构缺陷和额外的孔隙空间，从而增加了比表面积和孔体积。最后，通过与气相色谱-质谱联用（GC-MS），将涂覆有Am-UIO-66的SPME纤维成功应用于测定乳胶手套中亚硝胺的迁移，实现了良好的线性关系（20-2000ng/L）、令人满意的回收率（85.2-112.8%）和相当低的检测限（2.61-6.12ng/L）。
