以单质硫为固定相的薄层色谱-红外光谱技术

doi:10.7503/cjcu20130998

高等学校化学学报 ›› 2014, Vol. 35 ›› Issue (4): 741.doi: 10.7503/cjcu20130998

以单质硫为固定相的薄层色谱-红外光谱技术

范晓坤^1,², 姜叶^2,³, 石佳佳^1,², 刘翠格¹, 魏永巨¹(), 宋增福⁴, 翁诗甫², 杨展澜², 徐怡庄²(), 吴瑾光²

1. 河北师范大学化学与材料科学学院, 石家庄 050024
2. 北京大学化学与分子工程学院, 北京 100871
3. 辽宁中医药大学药学院, 大连 116600
4. 北京大学物理学院, 北京100871

收稿日期:2013-10-14 出版日期:2014-04-10 发布日期:2014-02-25
作者简介:联系人简介: 魏永巨, 男, 教授, 主要从事分子光谱分析和中药荧光分析等方面的研究. E-mail: weiyju@126.com ; 徐怡庄, 男, 博士, 副教授, 主要从事分子光谱的基础研究及其在材料和生命科学中的应用研究. E-mail: xyz@pku.edu.cn
基金资助:
国家自然科学基金(批准号: 501373003, 20975029, 81173496)资助

Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis^†

FAN Xiaokun^1,², JIANG Ye^2,³, SHI Jiajia^1,², LIU Cuige¹, WEI Yongju^1,^*(), SONG Zengfu⁴, WENG Shifu², YANG Zhanlan², XU Yizhuang^2,^*(), WU Jinguang²

1. College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024, China
2. College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China
3. College of Pharmacy, Liaoning University of Traditional Chinese Medicine, Shenyang 116600, China
4. College of Physics, Peking University, Beijing 100871, China

Received:2013-10-14 Online:2014-04-10 Published:2014-02-25
Contact: WEI Yongju,XU Yizhuang E-mail:weiyju@126.com;xyz@pku.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(Nos.501373003, 20975029, 81173496)

摘要/Abstract

摘要：

以中红外光透明的单质硫作为薄层色谱的新型固定相. 减小固定相颗粒大小有助于分离, 因此通过优化实验条件制备了粒径约为500 nm的硫颗粒, 并用其制备了普通的薄层板和窄带薄层板以开展原位薄层色谱-红外光谱联用分析. 以罗丹明B和龙胆紫以及罗丹明B和溴酚蓝为研究对象, 实验结果表明, 以单质硫作为新型固定相的薄层板具备一定的分离混合组分的能力, 且不影响分离组分的红外检测, 可以实现薄层色谱-红外光谱联用分析.

关键词: 薄层色谱, 红外光谱, 硫, 窄带薄层板

Abstract:

In situ thin-layer chromatography-Fourier transform infrared spectroscopy(TLC-FTIR) technique has tremendous potential in the analysis of complex mixtures. However, the progress in this technique was quite slow. The reason is that conventional stationary phase has strong absorption in FTIR spectrum and brings about severe interference in the detection of samples. This paper proposes to use sulfur fine particles, which is transparent in mid-infrared, as a new type of TLC stationary phase. Additionally, decreasing the particle size of sulfur is very important in TLC-FTIR analysis technique. By optimizing the experimental conditions, the sulfur particle with a size of 500 nm was prepared and the conventional TLC plate and the narrow TLC plate using the sulfur paticles as the stationary phase was prepared. TLC experimental results prove that the TLC plate can separate the mixture of rhodamine B and gentian violet successfully. FTIR analysis confirms that the FTIR spectra of the separated rhodamine B/gentian violet spots and rhodamine B/bromophenol blue spots are in good agreement with the FTIR spectra of pure rhodamine B, gentian violet and bromophenol blue.

Key words: Thin-layer chromatography, Fourier transform infrared spectroscopy(FTIR), Sulfur, Narrow-band thin-layer chromatography(TLC) plate

中图分类号:

O657

TrendMD:

范晓坤, 姜叶, 石佳佳, 刘翠格, 魏永巨, 宋增福, 翁诗甫, 杨展澜, 徐怡庄, 吴瑾光. 以单质硫为固定相的薄层色谱-红外光谱技术. 高等学校化学学报, 2014, 35(4): 741.

FAN Xiaokun, JIANG Ye, SHI Jiajia, LIU Cuige, WEI Yongju, SONG Zengfu, WENG Shifu, YANG Zhanlan, XU Yizhuang, WU Jinguang. Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis^†. Chem. J. Chinese Universities, 2014, 35(4): 741.

图/表 7

Fig.1 XRD pattern of the product by the reaction between sodium thiosulfate and hydrochloric acid(A) and standard XRD pattern of sulfur particles(B)

Fig.2 FTIR spectrum of the sulfur particles

Fig.3 SEM image of the sulfur particles

Fig.4 Photographs of a traditional TLC plate(A) and a narrow-band TLC plate(B)

Fig.5 Photograph of a narrow-band TLC plate using sulfur particles as stationary phase to separate the mixture of rhodamine B and gentian violet(A) and the mixture of rhodamine B and bromophenol blue(B) after chromatographic experiment

Fig.6 FTIR spectra of gentian violet(A) and rhodamine B(B) on the sulfur narrow-band TLC plateMass fraction of sample: a. 100%; b. 0.5%; c. 0.2%; d. 0.1%. Mobile phase: tetrahydrofuran, methanol and ammonia water.

Fig.7 FTIR spectra of bromophenol blue(A) and rhodamine B(B) on the sulfur narrow-band TLC plate a. Pure sample; b. 0.2%(mass fraction) sample. Mobile phase: ethyl acetate, methanol and ammonia water.

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以单质硫为固定相的薄层色谱-红外光谱技术

Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis^†

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以单质硫为固定相的薄层色谱-红外光谱技术

Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis†

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Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis^†