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Thin-layer chromatographic plate and TLC (thin-layer chromatography)-infrared spectrography coupled combined method using same

A technology of thin-layer chromatography plate and infrared spectroscopy, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of slow progress, low sensitivity of thin-layer chromatography-infrared technology, and achieve the effect of high sensitivity

Inactive Publication Date: 2013-08-14
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the attempt to combine thin-layer chromatography with infrared spectroscopy has been reported in the literature, the technology has been slow for a long time. The main reason is that the stationary phases used in traditional thin-layer chromatography separation techniques such as silica gel, oxidation Aluminum, cellulose, and polyamide all have strong infrared absorption. This kind of infrared absorption signal will strongly cover the infrared absorption signal of the sample, resulting in low sensitivity of thin-layer chromatography-infrared chromatography, so it is difficult to obtain practical application

Method used

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  • Thin-layer chromatographic plate and TLC (thin-layer chromatography)-infrared spectrography coupled combined method using same
  • Thin-layer chromatographic plate and TLC (thin-layer chromatography)-infrared spectrography coupled combined method using same
  • Thin-layer chromatographic plate and TLC (thin-layer chromatography)-infrared spectrography coupled combined method using same

Examples

Experimental program
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Effect test

Embodiment 1

[0051] The preparation of embodiment 1 barium fluoride nanopowder

[0052] Weigh 31 grams of Ba(OH) 2 Solid (analytically pure), it is dissolved in water-ethanol mixed liquid (volume ratio 1:1) to make a saturated solution. While stirring, slowly drop in HF aqueous solution until the solution is neutral. Centrifuge the obtained precipitated turbid liquid to remove the aqueous solution, then wash and centrifuge with deionized water, check whether HF still exists in the precipitate with pH test paper, wash and centrifuge until the pH test paper is neutral. Then the washed precipitate was transferred into a porcelain crucible and placed in a muffle furnace, and dried at 300°C.

[0053] The obtained dry BaF 2 Precipitate particles, fix on the sample stage with conductive glue, carry out vacuum gold spraying treatment according to the operating instructions of the following scanning electron microscope, and observe the particle size of the sample with a scanning electron microsc...

Embodiment 2

[0061] Embodiment 2 The preparation of barium fluoride layer as the chromatographic plate of adsorbent layer

[0062] Weigh 0.5 g of the barium fluoride prepared in the examples, add it into 40 ml of water, form a suspension by shaking and stirring, then add the above suspension into a beaker with a 1.5 cm × 3 cm barium fluoride single chip, and place it on the beaker mouth Place a piece of filter paper and let it stand in a fume hood for 3 days, so that the barium fluoride particles slowly settle on the barium fluoride single wafer (produced by Beijing Glass Research Institute) substrate, until the water evaporates completely, and a chromatographic plate is obtained.

[0063] Gained chromatographic plate in embodiment 2 in embodiment 3 carries out thin-layer chromatography test

[0064] (1) Take 0.025 grams of methylene blue and rhodamine B respectively, dissolve them with 15 milliliters of anhydrous methanol, and make a mixed solution. : 5 ml of ethyl acetate: 1 ml of dieth...

Embodiment 4

[0066] Embodiment 4 cuprous iodide is as the preparation of the chromatographic plate of adsorbent

[0067] Except using cuprous iodide powder instead of barium fluoride powder, using 50ml of water, and using 1.5cm×3cm silicon single wafer instead of barium fluoride single wafer, obtain cuprous iodide as adsorbent in the same manner as in Example 2 chromatography plate.

[0068] Gained chromatographic plate in embodiment 6 embodiment 4 carries out thin-layer chromatography test

[0069] Carry out thin-layer chromatography test similarly with the mode of embodiment, the result is similar to the result in embodiment 3.

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Abstract

The invention relates to a thin-layer chromatographic plate and a TLC (thin-layer chromatography)-infrared spectrography coupled method using the same. In the TLC separation and mid-infrared spectrum detection coupled method, the thin-layer chromatographic plate comprises a chromatographic-plate substrate and an adsorbent layer, wherein the adsorbent layer is formed on the chromatographic-plate substrate; the chromatographic-plate substrate is a substrate without mid-infrared absorption or a mid-infrared reflective substrate; the adsorbent layer is prepared from one or more types of adsorbents selected from mid-infrared specular insoluble nonabsorbent inorganic metal salts; and the chromatographic plate is used as a sample substrate for infrared spectroscopy detection.

Description

technical field [0001] The invention relates to a combined method of thin-layer chromatography and infrared spectroscopy, in particular to a novel combined method of thin-layer chromatography and infrared spectroscopy. Background technique [0002] Thin-layer chromatography is a liquid chromatography technique, which usually uniformly coats the stationary phase on the surface of glass, metal or plastic to form a thin layer, and then places the sample on one end of the thin layer, and the mobile phase flows through capillary action. Through the stationary phase, the effective separation of the sample can be achieved. Thin-layer chromatography is widely used in qualitative detection of target substances, selection of chromatographic column conditions, detection of compound purity, quantitative analysis, tracking and monitoring of organic compound synthesis, drug analysis and content determination, etc. [0003] However, the traditional thin-layer chromatography separation met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/92G01N30/93G01N30/95
Inventor 潘庆华丁洁王满满刘溪李晓佩孙燕来国桥余江周风山翁诗甫龚蓉烨高学军刘志国武惠忠张元福魏永巨刘翠格李维红杨展澜徐怡庄吴瑾光
Owner PEKING UNIV