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基于碳纳米管增强中空纤维固/液微萃取的新型提取技术,结合高效液相色谱法测定吡罗昔康和双氯芬酸。

A novel extraction technique based on carbon nanotubes reinforced hollow fiber solid/liquid microextraction for the measurement of piroxicam and diclofenac combined with high performance liquid chromatography.

机构信息

Key Laboratory of Chemistry of Northwestern Plant Resources, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, PR China.

出版信息

Talanta. 2012 Oct 15;100:153-61. doi: 10.1016/j.talanta.2012.08.042. Epub 2012 Sep 3.

Abstract

A novel design of carbon nanotubes reinforced hollow fiber solid/liquid phase microextraction (CNTs-HF-SLPME) was developed to determine piroxicam and diclofenac in different real water samples. Functionalized multi-walled carbon nanotubes (MWCNTs) were held in the pores of hollow fiber with sol-gel technology. The pores and lumen of carbon nanotubes reinforced hollow fiber were subsequently filled with a μL volume of organic solvent (1-octanol), and then the whole assembly was used for the extraction of the target analytes in direct immersion sampling mode. The target analytes were extracted from the sample by two extractants, one of which is organic solvent placed inside the pores and lumen of hollow fiber and the other one is CNTs held in the pores of hollow fiber. After extraction, the analytes were desorbed in acetonitrile and analyzed using high performance liquid chromatography. This novel extraction mode showed more excellent extraction performance in comparison with conventional hollow fiber liquid microextraction (without adding CNTs) and carbon nanotubes reinforced hollow fiber solid microextraction (CNTs held in the pores of hollow fiber, but no organic solvents placed inside the lumen of hollow fiber) under the respective optimum conditions. This method provided 47- and 184-fold enrichment factors for piroxicam and diclofenac, respectively, good inter-fiber repeatability and batch-to-batch reproducibility. Linearity was observed in the range of 20-960 μg L(-1) for piroxicam, and 10-2560 μg L(-1) for diclofenac, with correlation coefficients of 0.9985 and 0.9989, respectively. The limits of detection were 4.58 μg L(-1) for piroxicam and 0.40 μg L(-1) for diclofenac.

摘要

一种新型的碳纳米管增强中空纤维固/液相微萃取(CNTs-HF-SLPME)被设计用于在不同的实际水样中测定吡罗昔康和双氯芬酸。功能化多壁碳纳米管(MWCNTs)通过溶胶-凝胶技术固定在中空纤维的孔中。随后,将有机溶剂(1-辛醇)μL 体积填充到碳纳米管增强中空纤维的孔和内腔中,然后整个组件用于直接浸入采样模式下目标分析物的萃取。目标分析物通过两种萃取剂从样品中萃取出来,一种是置于中空纤维孔和内腔中的有机溶剂,另一种是置于中空纤维孔中的碳纳米管。萃取后,在乙腈中解吸分析物,并使用高效液相色谱法进行分析。在各自的最佳条件下,与传统的中空纤维液相微萃取(不添加 CNTs)和碳纳米管增强中空纤维固相微萃取(CNTs 置于中空纤维的孔中,但内腔中未放置有机溶剂)相比,这种新型的萃取模式表现出更好的萃取性能。该方法分别为吡罗昔康和双氯芬酸提供了 47 倍和 184 倍的富集因子,具有良好的纤维间重现性和批间重现性。吡罗昔康的线性范围为 20-960μg/L,相关系数为 0.9985;双氯芬酸的线性范围为 10-2560μg/L,相关系数为 0.9989。吡罗昔康的检测限为 4.58μg/L,双氯芬酸的检测限为 0.40μg/L。

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