Preparation and application of thin-layer chromatographic plate

Abstract

The invention discloses preparation and application of a thin-layer chromatography plate, and the preparation comprises the following steps: dispersing thin-layer chromatography silica gel in ethanol, and adding a silane coupling agent and an acid catalyst to obtain modified silica gel; respectively dissolving sodium carboxymethyl cellulose and polyvinyl alcohol in water, and mixing to obtain an adhesive solution; and uniformly mixing the modified silica gel and an adhesive by using a high-speed dispersion machine, coating a glass plate with the mixture, drying and activating. The prepared thin-layer chromatography plate is flat in plate surface, free of cracking and delaminating, good in separation effect and obvious in color development, and has a very good application prospect in the aspect of detection and analysis of flavors, fragrances and related substances.

Description

Technical Field

[0001] The invention relates to the field of chemical analysis, in particular to the preparation and application of a thin layer chromatography plate used in a chemical component identification thin layer chromatography method. Background Art

[0002] Thin layer chromatography plates are prepared by coating a mixture of adsorbents and adhesives on a plate. They are a detection method for separation, qualitative and quantitative analysis of mixed samples. Commonly used adsorbents for thin layer chromatography plates are various silica gels (silica gel G, silica gel GF-254, silica gel H, silica gel HF-254, etc.), alumina, cellulose, polyamide, etc.; commonly used adhesives are mainly sodium carboxymethyl cellulose, starch and its derivatives, etc.; commonly used plates are mainly glass plates, aluminum plates, plastic plates, etc.

[0003] Due to the characteristics of easy operation, small sample loading, and fast speed, thin layer chromatography plates have been widely used in the fields of medicine, chemical industry, biochemistry, environmental protection, etc. for qualitative or quantitative detection of certain substances. However, existing thin layer chromatography plates still have problems such as weak separation effect and poor color development effect for some highly polar substances. Therefore, by changing the adsorbent or adhesive, it is expected to obtain a thin layer chromatography plate with a smooth and delicate surface, better separation effect, and obvious color development, which is of great significance for the detection and analysis of flavors and related substances. Summary of the invention

[0004] Based on the above deficiencies in the prior art, the technical problem solved by the present invention is to provide a method for preparing a thin layer chromatography plate with a smooth and delicate surface, good separation effect and obvious color development, in view of the fact that the existing thin layer chromatography plates have weak separation effect and poor color development effect on highly polar substances. The plate can be applied to the detection and analysis of flavors and fragrances and related substances.

[0005] In order to solve the above technical problems, the present invention provides a preparation method of a thin layer chromatography plate, comprising the following steps:

[0006] Disperse thin layer chromatography silica gel in ethanol, add silane coupling agent and concentrated hydrochloric acid, reflux reaction, filter, and vacuum dry to obtain modified silica gel; dissolve sodium carboxymethyl cellulose and polyvinyl alcohol in water to obtain sodium carboxymethyl cellulose solution and polyvinyl alcohol solution respectively, mix the sodium carboxymethyl cellulose solution and the polyvinyl alcohol solution to obtain an adhesive; mix the modified silica gel and the adhesive evenly and apply them on a glass plate, dry, and activate to obtain a thin layer chromatography plate.

[0007] As a preferred embodiment of the above technical solution, the preparation of the thin layer chromatography plate provided by the present invention further includes part or all of the following technical features:

[0008] As an improvement of the above technical solution, the thin layer chromatography silica gel is 200-300 mesh, and the manufacturer is preferably Qingdao Ocean Chemical.

[0009] As an improvement of the above technical solution, the silane coupling agent is hexamethyldisiloxane or n-octyltriethoxysilane.

[0010] As an improvement of the above technical solution, the mass ratio of the silane coupling agent to the thin layer chromatography silica gel is 5-20%.

[0011] As an improvement of the above technical solution, the alcoholysis degree of the polyvinyl alcohol is 78.5-81.5 mol% or 86.5-89.0 mol%.

[0012] As an improvement of the above technical solution, the mass concentration of the solution after the sodium carboxymethyl cellulose and polyvinyl alcohol are mixed is 0.5% to 1.5%.

[0013] As an improvement of the above technical solution, the mass ratio of sodium carboxymethyl cellulose to polyvinyl alcohol is 2:1, 1:1 or 1:2.

[0014] As an improvement of the above technical solution, the mass ratio of the adhesive to the modified silica gel is 1% to 2%.

[0015] The present invention also provides the use of any of the above-mentioned thin layer chromatography plates, characterized in that the thin layer chromatography plate is used for the detection and analysis of flavors and fragrances and related substances.

[0016] As an improvement of the above technical solution, the thin layer chromatography plate is applied to the detection and analysis of flavors and fragrances 180, flavors and fragrances 2101, artemisia essential oil and related substances.

[0017] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0018] (1) By modifying the thin layer chromatography silica gel, the separation effect of highly polar substances can be improved and more sample components can be analyzed;

[0019] (2) The color development effect of thin layer chromatography spots can be improved by adjusting the ratio of sodium carboxymethyl cellulose and polyvinyl alcohol as the adhesive;

[0020] (3) The present invention can be widely used in the detection and analysis of flavors and fragrances and related substances in the pharmaceutical chemical industry, food testing, biotechnology and other industries.

[0021] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present invention more obvious and easy to understand, the following is a detailed description in combination with the preferred embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.

[0023] Figure 1 (a) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared in a comparative example of the present invention under the polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0024] Figure 1 (b) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on a thin layer chromatography plate in Example 1 of the present invention at a polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0025] Figure 1 (c) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on a thin layer chromatography plate in Example 2 of the present invention at a polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0026] Figure 1 (d) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on a thin layer chromatography plate in Example 3 of the present invention at a polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0027] Figure 1 (e) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on a thin layer chromatography plate in Example 4 of the present invention at a polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0028] Figure 1 (f) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on a thin layer chromatography plate in Example 5 of the present invention at a polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil;

[0029] Figure 1 (g) is a thin layer chromatogram of flavors and fragrances 180 / 2101 and mugwort essential oil prepared on the thin layer chromatography plate in Example 6 of the present invention under the polarity of methanol: water: acetic acid = 5:1:1, and the spots from left to right are flavors and fragrances 180, flavors and fragrances 2101 and mugwort essential oil, respectively. DETAILED DESCRIPTION

[0030] The specific implementation modes of the present invention are described in detail below, which is a part of this specification. The principles of the present invention are explained through examples. Other aspects, features and advantages of the present invention will become clear through the detailed description.

[0031] Example 1

[0032] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of hexamethyldisiloxane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 78.5-81.5mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 15mL of sodium carboxymethyl cellulose solution and 15mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive evenly with a high-speed disperser and apply it on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0033] Example 2

[0034] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of hexamethyldisiloxane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 86.5-89.0mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 15mL of sodium carboxymethyl cellulose solution and 15mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive evenly with a high-speed disperser and apply it on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0035] Example 3

[0036] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of n-octyltriethoxysilane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 78.5-81.5mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 15mL of sodium carboxymethyl cellulose solution and 15mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive evenly with a high-speed disperser and apply it on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0037] Example 4

[0038] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of n-octyltriethoxysilane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 86.5-89.0mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 15mL of sodium carboxymethyl cellulose solution and 15mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive evenly with a high-speed disperser and apply it on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0039] Example 5

[0040] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of n-octyltriethoxysilane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 78.5-81.5mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 20mL of sodium carboxymethyl cellulose solution and 10mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive evenly with a high-speed disperser and apply it on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0041] Example 6

[0042] Disperse 15g of thin layer chromatography silica gel in 50mL of ethanol, add 1.5g of n-octyltriethoxysilane and 50μL of concentrated hydrochloric acid, reflux for 8h, then filter and vacuum dry to obtain modified silica gel; dissolve 1g of sodium carboxymethyl cellulose and 1g of polyvinyl alcohol (degree of alcoholysis: 78.5-81.5mol%) in 200mL of water respectively, heat to 90°C, stir to dissolve, take 10mL of sodium carboxymethyl cellulose solution and 20mL of polyvinyl alcohol solution respectively and mix to obtain 30mL of adhesive solution; then mix 10g of modified silica gel and 30mL of adhesive using a high-speed disperser and apply them on a glass plate, dry naturally, and activate in a 100°C forced air drying oven for 30min to obtain a thin layer chromatography plate.

[0043] Test example

[0044] Comparative Example: Dissolve 1 g of sodium carboxymethyl cellulose in 200 mL of water, heat to 90°C, and stir to dissolve; then mix 10 g of thin layer chromatography silica gel and 30 mL of sodium carboxymethyl cellulose solution evenly using a high-speed disperser and apply it on a glass plate, dry it naturally, and activate it in a 100°C forced air drying oven for 30 minutes to obtain a thin layer chromatography plate.

[0045] Thin layer chromatography plate test: 2 μL of flavors and fragrances 180 / 2101 and mugwort essential oil were drawn with a capillary tube and spotted on the thin layer chromatography plates prepared in Examples 1-6, respectively, with methanol: water: acetic acid = 5:1:1 as the developing solvent, developed, taken out, dried, stained with iodine staining and observed under a 254 nm ultraviolet lamp. The adhesion, surface fineness, separation ability and color development effect of the thin layer chromatography plate were tested. The results are shown in Table 1 and the thin layer chromatogram is shown in Figure 1 .

[0046] Table 1 Adhesion, surface fineness, separation ability and color development effect of thin layer chromatography plates

[0047]

[0048] As can be seen from Table 1, modifying silica gel with a silane coupling agent and replacing the adhesive can improve the separation and color development effect of the thin layer plate on flavors and fragrances. Most of the thin layer chromatography plates prepared by the present invention have better separation ability and color development effect than the comparative examples, among which Example 3 has the best comprehensive effect, no silica gel falls off during the development process, the surface of the thin layer plate is smooth and delicate, and has the best separation ability and color development effect.

[0049] from Figure 1 It can be seen that Example 1 Figure 1 (b) Embodiment 2 Figure 1 (c) Embodiment 3 Figure 1 (d) Embodiment 5 Figure 1 (f) No silica gel falls off during the development process, the water resistance is good, and the separation effect and color development effect are better than the comparative example Figure 1 (a) Example 3 Figure 1 (d) has the best comprehensive effect. No silica gel falls off during the development process, the surface of the thin layer plate is smooth and delicate, and the separation ability and color development effect are the best.

[0050] The raw materials listed in the present invention, as well as the upper and lower limits and interval values ​​of the raw materials of the present invention, and the upper and lower limits and interval values ​​of the process parameters (such as temperature, time, etc.) can all realize the present invention, and the embodiments are not listed one by one here.

[0051] The above is only a preferred embodiment of the present invention, which certainly cannot be used to limit the scope of rights of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and changes can be made without departing from the principle of the present invention, and these improvements and changes are also regarded as the protection scope of the present invention.

Claims

1. A method for preparing a thin layer chromatography plate, characterized in that: The following steps are included: Dispersing thin layer chromatography silica gel in ethanol, adding silane coupling agent and concentrated hydrochloric acid, reflux reaction, suction filtration, vacuum drying to obtain modified silica gel; dissolving sodium carboxymethyl cellulose and polyvinyl alcohol in water to obtain sodium carboxymethyl cellulose solution and polyvinyl alcohol solution respectively, mixing the sodium carboxymethyl cellulose solution and the polyvinyl alcohol solution to obtain an adhesive; The modified silica gel and the adhesive are mixed evenly and coated on a glass plate, dried and activated to obtain a thin layer chromatography plate.

2. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The thin layer chromatography silica gel has a mesh size of 200 to 300.

3. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The silane coupling agent is hexamethyldisiloxane or n-octyltriethoxysilane.

4. The preparation of the thin layer chromatography plate according to claim 2, characterized in that: The mass ratio of the silane coupling agent to the thin layer chromatography silica gel is 5-20%.

5. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The alcoholysis degree of the polyvinyl alcohol is 78.5-81.5 mol % or 86.5-89.0 mol %.

6. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The mass concentration of the solution after the sodium carboxymethyl cellulose and polyvinyl alcohol are mixed is 0.5% to 1.5%.

7. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The mass ratio of the sodium carboxymethyl cellulose to the polyvinyl alcohol is 2:1, 1:1 or 1:

2.

8. The preparation of the thin layer chromatography plate according to claim 1, characterized in that: The mass ratio of the adhesive to the modified silica gel is 1% to 2%.

9. The use of a thin layer chromatography plate as claimed in any one of claims 1 to 8, characterized in that: The thin layer chromatography plate is used for the detection and analysis of flavors and fragrances and related substances.

10. Use of the thin layer chromatography plate according to claim 9, characterized in that: The thin layer chromatography plate is applied to the detection and analysis of flavors and fragrances 180, flavors and fragrances 2101, mugwort essential oil and related substances.

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