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Narrow band thin-layer chromatographic sheet and preparation method thereof

A thin-layer chromatographic plate and thin-layer chromatography technology, which is used in instruments, measuring devices, scientific instruments, etc., can solve the problem that the preparation time of thin-layer plates affects large-scale use, the preparation time of thin-layer plates is long, and the development of thin-layer chromatography is affected. problem, to achieve the effect of convenient infrared detection, low cost, and improved detection sensitivity

Inactive Publication Date: 2014-12-24
PEKING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the case of a small spot sample, due to the influence of spot diffusion and tailing after TLC separation, it was found in the experiment that when the sample concentration is lower than 0.5%, the components separated by TLC cannot be detected by infrared light. Detected, this weakness also affected the development of thin-layer chromatography and infrared spectroscopy;
[0011] (3) The preparation time of thin-layer board is long
To a certain extent, the long preparation time of TLC will affect its large-scale use
In addition, the use of a large number of separate liquids may cause pollution problems and potential safety hazards in the future large-scale production process

Method used

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  • Narrow band thin-layer chromatographic sheet and preparation method thereof
  • Narrow band thin-layer chromatographic sheet and preparation method thereof
  • Narrow band thin-layer chromatographic sheet and preparation method thereof

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preparation example Construction

[0044] According to another aspect of the present invention, a kind of preparation method of narrow-band thin-layer chromatography plate is provided, and the method comprises:

[0045] (1) Grinding the stationary phase material into fine powder,

[0046] (2) Mix the stationary phase fine powder with the dispersion liquid to form a suspension under the action of ultrasonic waves,

[0047] (3) Feed the suspension into the flat groove on the chromatographic substrate, and obtain a narrow-band thin-layer chromatographic plate after the dispersion liquid evaporates.

[0048] In the preparation method of the narrow-band thin-layer chromatography plate according to the present invention, ethanol and water can be used as the dispersion liquid.

[0049] In the narrow-band thin-layer chromatography plate preparation method according to the present invention, ultrasonic waves help to form a uniform suspension in a short time.

[0050] In the preparation method of the narrow-band thin-l...

Embodiment 1

[0055] Open two straight grooves on the glass thin-layer plate. The width of the groove is 1mm and the depth is about 110μm. In a weighing bottle, ultrasonically treat it for 2 minutes to form a thicker suspension. After standing still for 2 minutes, transfer the upper suspension to another weighing bottle, and add the suspension to the groove of the glass thin-layer plate. In the process, after ethanol volatilizes (about 20 minutes), use a glass slide to push flatly on the surface of the thin-layer plate in the same direction to remove the silver iodide remaining near the groove, and obtain a narrow-band thin-layer chromatography plate with a flat surface, as shown in Figure 1 Show.

[0056] Previously, the "sedimentation and volatilization method" was used to prepare thin-layer plates, and more ethanol was added, and it took about three days to completely volatilize, but it only took about 0.5 hours to implement this preparation method; on the other hand, the amount of stati...

Embodiment 2

[0057] Thin-layer chromatography-infrared spectrum application of embodiment 2 narrow-band thin-layer chromatography plate

[0058] Weigh 0.1g rhodamine B and 0.1g bromocresol green respectively in a weighing bottle, add 10ml absolute ethanol respectively to prepare 1% rhodamine B pure product solution and 1% bromocresol green pure product solution; and then respectively prepared into 0.5%, 0.2%, 0.1% rhodamine B and bromocresol green mixed solution.

[0059] Firstly spot 1% pure Rhodamine B and measure the reflectance infrared spectrum, then use 0.5%, 0.2%, and 0.1% mixed samples to spot the sample respectively, the developing agent is V 乙醇 :V 乙酸乙酯 :V 氨水 =25:15:1, after development, the complete separation of bromocresol green and rhodamine B, the narrow-band TLC plate after separation is as figure 2 As shown, it can be seen that the spots of the separated samples are smaller and the samples are completely separated.

[0060] Dry the separated TLC at 120°C for 2 h, cool ...

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Abstract

The invention relates to a narrow band thin-layer chromatographic sheet which comprises a base plate. A straight groove is arranged on the chromatograph base plate, a fixed phase is precipitated in the straight groove, and fixed phase substances are selected from silver iodide, barium fluoride, calcium fluoride, silver bromide or zinc sulfide. The fixed phase of the chromatographic sheet is small in consumption, the cost is low, the detection sensitivity is high, the plating time is short, and the usage is convenient.

Description

technical field [0001] The invention relates to the combined use technology of thin-layer chromatography and infrared spectrum, in particular to narrow-band thin-layer chromatography which can be combined with red spectrum and a preparation method thereof. Background technique [0002] Thin layer chromatography is a fast, simple, efficient, economical and widely used chromatographic analysis method. It has great advantages in separating different components of a mixture, but there are certain limitations in the detection and identification of unknown components after separation. Limitations; while infrared spectroscopy can help identify organic functional groups, with the help of fingerprints and a large infrared spectrum database, the unknown components after thin-layer chromatography separation are identified. The combination of the two will greatly improve the ability to analyze complex mixtures. It is an analytical technique with broad application prospects and worthy of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/92
Inventor 王方李晓佩吴海军祝青魏永巨刘翠格翟延君徐怡庄吴瑾光
Owner PEKING UNIV
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