阅读说明：本技术 一种硝酸舍他康唑乳膏的鉴别方法 (Identification method of sertaconazole nitrate cream ) 是由 韦家华 刘玉 于 2020-12-31 设计创作，主要内容包括：本发明提供一种硝酸舍他康唑乳膏的鉴别方法,包括：(1)取硝酸舍他康唑乳膏样品,加入无水乙醇,水浴中加热溶解,离心,取上清液作为供试品溶液；(2)取硝酸舍他康唑对照品,加入无水乙醇溶解,稀释,作为对照品溶液；(3)采用三氯甲烷、正已烷、甲醇和浓氨溶液混合为展开剂1；采用正辛醇、乙酸乙酯：丙酮混合为展开剂2；(4)各1～2μl,分别点于同一硅胶GF-(254)薄层板上,依次置于展开剂1和展开剂2中展开,晾干,置于紫外灯254nm下检视,本发明的鉴别方法可缩短硅胶GF-(254)薄层板的活化时间,斑点明显清晰,且分离稳定,不拖尾,Rf值适中,对硝酸舍他康唑乳膏的薄层色谱法鉴别具有良好的重复性和稳定性。(The invention provides an identification method of sertaconazole nitrate cream, which comprises the following steps: (1) taking a sertaconazole nitrate cream sample, adding absolute ethyl alcohol, heating and dissolving in a water bath, centrifuging, and taking supernate as a test sample solution; (2) taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol for dissolving, and diluting to obtain a reference substance solution; (3) mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution to obtain a developing agent 1; adopting n-octanol and ethyl acetate: mixing acetone to obtain a developing agent 2; (4) 1-2 mul each, respectively dropping on the same silica gel GF 254 The thin layer plate is sequentially placed in a developing agent 1 and a developing agent 2 for development, air-dried and placed under an ultraviolet lamp at 254nm for inspection, and the identification method can shorten the GF of the silica gel 254 The activation time of the thin layer plate is obvious and clear, the separation is stable, no tailing is caused, the Rf value is moderate, and the nitric acid sertacon is obtainedThe thin layer chromatography identification of the oxazole cream has good repeatability and stability.)

1. The identification method of the sertaconazole nitrate cream is characterized by comprising the following steps: the method comprises the following steps:

(1) preparing a test solution: taking a sertaconazole nitrate cream sample, adding absolute ethyl alcohol, heating and dissolving in a water bath, cooling, centrifuging, and taking a supernatant as a test sample solution; the mass concentration of the test solution is (0.8-1.2) mg/ml;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the sertaconazole nitrate reference substance to prepare a sertaconazole nitrate solution with the mass concentration of (0.8-1.2) mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution according to the mass ratio of (45-55): 40-60): 15-25): 1-3 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: acetone (60-70): (20-30): (5-15) mixing to obtain a developing agent 2;

(4) chromatographic conditions and manipulationsThe method comprises the following steps: according to the thin layer chromatography, sucking 1-2 μ l of each of the sample solution and the reference solution, and respectively dropping on the same silica gel GF₂₅₄And (3) sequentially placing the thin-layer plate in a developing agent 1 and a developing agent 2 for development, taking out, airing, placing under an ultraviolet lamp at 254nm, and inspecting the positions and colors of main spots displayed by the test solution and the reference solution.

2. A method of identifying sertaconazole nitrate cream according to claim 1, characterized in that: in the step 1, the water bath heating temperature is 65-75 ℃, the centrifugal speed is 2000-3000 r/min, and the separation time is 3-5 min.

3. A method of identifying sertaconazole nitrate cream according to claim 2, characterized in that: in the step 1, after centrifugal treatment, taking supernatant, adding equal volume of absolute ethyl alcohol again, mixing, performing ultrasonic treatment for 10-15 min, and filtering to obtain a test solution.

4. A method of identifying sertaconazole nitrate cream according to claim 3, characterized in that: preparing a negative sample control solution, namely preparing the negative sample control solution by taking a cream auxiliary material which does not contain sertaconazole nitrate according to the preparation method of the test sample solution;

step 4, sucking 1-2 mul of negative sample control solution, and respectively dropping the negative sample control solution, the sample solution and the control solution on the same silica gel GF₂₅₄And (3) sequentially placing the thin-layer plate in a developing agent 1 and a developing agent 2, developing, taking out, airing, and placing under an ultraviolet lamp at 254nm for inspection to verify the negative sample interference effect.

5. A method of identifying sertaconazole nitrate cream according to any one of claims 1 to 4, characterized in that: the developing agent 1 is formed by mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution in a mass ratio of 50:50:20: 2; the developing agent 2 is formed by mixing trichloromethane, n-hexane and methanol according to a mass ratio of 65:25: 10.

6. A method of identifying sertaconazole nitrate cream according to claim 5, characterized in that: in step 4, silica gel GF₂₅₄Placing the thin layer in a developing agent 1, wherein the temperature of the developing agent 1 is 100-120 ℃, and placing the silica gel GF₂₅₄The thin layer is placed in a developing agent 2, and the temperature of the developing agent 2 is 95-105 ℃.

7. A method of identifying sertaconazole nitrate cream according to any one of claims 1 to 4, characterized in that: in step 4, the silica gel GF₂₅₄The thin-layer plate is activated in the developing agent 1 for 15-20 min and in the developing agent 2 for 6-10 min.

8. A method of identifying sertaconazole nitrate cream according to claim 7, characterized in that: in step 4, silica gel GF₂₅₄Taking out the thin-layer plate, drying the thin-layer plate by hot air at 60-80 ℃, immediately spraying an aluminum chloride solution with the mass concentration of 0.1-0.5% on the surface, and continuously drying at 100 ℃.

Technical Field

The invention relates to the technical field of medicines, in particular to an identification method of sertaconazole nitrate cream.

Background

Sertaconazole nitrate is a novel, broad-spectrum and efficient local antifungal agent, is developed and developed by Ferrer Spanish company, is firstly marketed in Spain in 1992, and is annotated in China in 2003 to be marketed as an ointment preparation. Compared with other clinical imidazole antibacterial agents, the imidazole antibacterial agent has antibacterial activity on pathogenic bacteria, pathogenic yeasts, skin fungi, opportunistic pathogens, filamentous fungi, gram-positive bacteria, trichomonas bacteria and the like which cause skin and mucosa infection, and therefore has a wider safety range.

The sertaconazole nitrate cream is a common preparation formulation, and the main drug is compounded with a plurality of auxiliary materials such as an emulsifier, a humectant, a stabilizer and the like, so that the sertaconazole nitrate cream has good stability, the full dispersion and emulsification effects are ensured, and the phenomena of emulsion breaking, layering and the like are reduced. In the preparation process of sertaconazole nitrate and cream formulations, the identification method of sertaconazole nitrate medicines is usually used for identifying sertaconazole nitrate cream products, but the existing sertaconazole nitrate identification method cannot effectively control the quality of the sertaconazole nitrate cream formulations, is influenced by the sertaconazole nitrate cream formulations, is difficult to achieve efficient and stable identification of the sertaconazole nitrate cream product quality, and is not beneficial to control of production and quality guarantee of the sertaconazole nitrate cream and wide clinical safety application.

Disclosure of Invention

In view of this, the invention provides an identification method of sertaconazole nitrate cream.

The technical scheme of the invention is realized as follows:

the invention provides an identification method of sertaconazole nitrate cream, which comprises the following steps:

(1) preparing a test solution: taking a sertaconazole nitrate cream sample, adding absolute ethyl alcohol, heating and dissolving in a water bath, cooling, centrifuging, and taking a supernatant as a test sample solution; the mass concentration of the test solution is (0.8-1.2) mg/ml;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the solution to prepare a sertaconazole nitrate solution with the mass concentration of 1mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution according to the mass ratio of (45-55): 40-60): 15-25): 1-3 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: acetone (60-70): (20-30): (5-15) mixing to obtain a developing agent 2;

(4) chromatographic conditions and operation: according to the thin layer chromatography, sucking 1-2 μ l of each of the sample solution and the reference solution, and respectively dropping on the same silica gel GF₂₅₄And (3) sequentially placing the thin-layer plate in a developing agent 1 and a developing agent 2 for development, taking out, airing, placing under an ultraviolet lamp at 254nm, and inspecting the positions and colors of main spots displayed by the test solution and the reference solution.

The invention uses silica gel GF₂₅₄The thin layer plate is used as carrier, and the developing agent 1 and the developing agent 2 are used for developing treatment, so that the silica gel GF can be shortened₂₅₄The thin layer plate is activated in the developing solvent for a long time, and experience shows that spots are obvious and clear, the color development is consistent, the separation is stable, no tailing is caused, the specific shift value Rf is moderate, and the thin layer chromatography identification of the sertaconazole nitrate cream has good repeatability and stability.

Preferably, in the step 1, the water bath heating temperature is 65-75 ℃, the centrifugal speed is 2000-3000 r/min, and the separation time is 3-5 min.

Preferably, in the step 1, after the centrifugal treatment, the supernatant is taken, the same volume of absolute ethyl alcohol is added again for mixing, the ultrasonic treatment is carried out for 10-15 min, and the filtration is carried out to obtain the test solution. The preparation of the test solution is carried out by adopting water bath heating and ultrasonic treatment, which is beneficial to improving the stability and the full separation of the effective components in the test solution.

Preferably, the method further comprises the preparation of a negative sample control solution, wherein the negative sample control solution is prepared by taking a cream auxiliary material which does not contain the sertaconazole nitrate according to the preparation method of the test sample solution.

Preferably, in step 4, 1-2 μ l of negative sample control solution is aspiratedDropping the solution, the sample solution and the reference solution on the same silica gel GF₂₅₄And (3) sequentially placing the thin-layer plate in a developing agent 1 and a developing agent 2, developing, taking out, airing, and placing under an ultraviolet lamp at 254nm for inspection to verify the negative sample interference effect. The invention can also verify the interference effect of the negative sample by further preparing a negative sample control solution, which shows that the identification method has specificity and ensures the stable quality, safety and controllability of the sertaconazole nitrate.

Preferably, the developing agent 1 is formed by mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution in a mass ratio of 50:50:20: 2; the developing agent 2 is formed by mixing trichloromethane, n-hexane and methanol according to a mass ratio of 65:25: 10.

Preferably, in step 4, the silica gel GF₂₅₄Placing the thin layer in a developing agent 1, wherein the temperature of the developing agent 1 is 100-120 ℃, and placing the silica gel GF₂₅₄The thin layer is placed in a developing agent 2, and the temperature of the developing agent 2 is 95-105 ℃.

Preferably, in step 4, the silica gel GF₂₅₄The thin-layer plate is activated in the developing agent 1 for 15-20 min and in the developing agent 2 for 6-10 min.

Preferably, in step 4, the silica gel GF₂₅₄Taking out the thin-layer plate, drying the thin-layer plate by using hot air at 60-80 ℃, immediately spraying an aluminum chloride solution with the mass concentration of 0.1-0.5% on the surface of the thin-layer plate, and continuously drying the thin-layer plate at 100 ℃ to facilitate the color development and the margin of spots to be clearer.

Compared with the prior art, the invention has the beneficial effects that: the invention provides a method for identifying sertaconazole nitrate cream, which mainly adopts silica gel GF₂₅₄The thin layer plate is used as a carrier, and the thin layer plate is compounded by trichloromethane, n-hexane, methanol and concentrated ammonia solution as a developing agent 1 and n-octanol and ethyl acetate: acetone is mixed as the developing agent 2 for combination, which can greatly shorten the silica gel GF₂₅₄The activation time of the thin-layer plate in the developing agent can realize obvious and clear spots, consistent color development, stable separation, no tailing and effective control of a specific shift value Rf below 30min, namely the ratio of the distance from the origin to the center of the spots to the distance from the origin to the front edge of the solvent, the Rf value is moderate, the separation degree is good, and the resolution ratio of the thin-layer plate in the developing agent is goodThe thin-layer chromatography identification of the sertaconazole nitrate cream has good repeatability and stability.

Drawings

FIG. 1 is a thin layer identification map of sertaconazole nitrate cream of example 1 of the present invention;

in the figure, 1 is a reference sample, 2 is a test sample 1, 3 is a test sample 2, and 4 is a test sample 3.

Detailed Description

In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.

The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.

The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.

The invention adopts sertaconazole nitrate cream produced in the same batch as a test raw material, and identifies the effective components of sertaconazole nitrate by the following specific identification method. Wherein, the sertaconazole nitrate cream is a white cream, and comprises the following components: 2% of sertaconazole nitrate, 3.5% of glyceryl monostearate, 5.5% of octadecanol, 2% of liquid paraffin, 6% of white vaseline, 0% of tween-8010%, 9% of propylene glycol, 4% of glycerol, 0.1% of ethylparaben and the balance of water.

Example 1

The identification method of the sertaconazole nitrate cream comprises the following steps: the method comprises the following steps:

(1) preparing a test solution: respectively taking 10 groups of sertaconazole nitrate cream samples, respectively taking 16mg of each sertaconazole nitrate cream sample, adding 20ml of absolute ethyl alcohol, placing in a water bath at 65 ℃, heating to dissolve, cooling, centrifuging at 2000r/min for 3min, and taking supernate as a test solution;

(2) preparing a reference solution: taking a reference substance of sertaconazole nitrate, wherein the purity of the sertaconazole nitrate is more than 99.5%, adding absolute ethyl alcohol for dissolving, and diluting to prepare a sertaconazole nitrate solution with the mass concentration of 0.8mg/ml as the reference substance solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution according to the mass ratio of 45:40:15:1 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: acetone 60: 20: 5, mixing to obtain a developing agent 2;

(4) chromatographic conditions and operation: according to thin layer chromatography, sucking 1 μ l of each of the sample solution and the control solution, and spotting on the same silica gel GF₂₅₄Sequentially placing on the thin layer plate in 100 deg.C developing agent 1 for 15min, placing in 95 deg.C developing agent 2 for 6min, taking out, air drying, and inspecting under ultraviolet lamp 254 nm; the results show that: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the control solution, as shown in FIG. 1.

Example 2

The identification method of the sertaconazole nitrate cream comprises the following steps: the method comprises the following steps:

(1) preparing a test solution: respectively taking 10 groups of sertaconazole nitrate cream samples 30mg respectively, adding 25ml of absolute ethyl alcohol, heating and dissolving in a water bath at 75 ℃, cooling, centrifuging at 3000r/min for 5min, and taking supernatant as a test solution;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the sertaconazole nitrate reference substance to prepare a sertaconazole nitrate solution with the mass concentration of 1.2mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and concentrated ammonia solution according to the mass ratio of 55:60:25:3 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: 70 parts of acetone: 30: 15 to obtain a developing solvent 2;

(4) chromatographic conditions and operation: according to thin layer chromatography, sucking 2 μ l of each of the sample solution and the control solution, and spotting on the same silica gel GF₂₅₄Sequentially placing on the thin layer plate in 120 deg.C developing agent 1 for 20min, placing in 105 deg.C developing agent 2 for 10min, taking out, air drying, and inspecting under ultraviolet lamp 254 nm; the results show that: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the reference solution.

Example 3

The identification method of the sertaconazole nitrate cream comprises the following steps: the method comprises the following steps:

(1) preparing a test solution: respectively taking 20mg of each of 10 groups of sertaconazole nitrate cream samples, adding 20ml of absolute ethyl alcohol, heating and dissolving in a water bath at 60 ℃, cooling, centrifuging at 2500r/min for 4min, and taking supernatant as a test solution;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the sertaconazole nitrate reference substance to prepare a sertaconazole nitrate solution with the mass concentration of 1.0mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and a concentrated ammonia solution according to a mass ratio of 50:50:20:2 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: mixing acetone 65:25:10 to obtain a developing solvent 2;

(4) chromatographic conditions and operation: according to thin layer chromatography, sucking 1 μ l of each of the sample solution and the control solution, and spotting on the same silica gel GF₂₅₄Sequentially placing the thin-layer plate in a developing agent 1 at 110 ℃ for 16min, placing the thin-layer plate in a developing agent 2 at 60-80 ℃ for 8min, taking out, drying in the air, and placing the thin-layer plate under an ultraviolet lamp 254nm for inspection; the results show that: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the reference solution.

Example 4

The method for identifying sertaconazole nitrate cream of this example differs from that of example 3 in that: in the step 1, after centrifugal treatment, taking supernatant, adding absolute ethyl alcohol with the same volume again, mixing, performing ultrasonic treatment for 10min, and filtering to obtain a test solution.

Inspection at 254nm under an ultraviolet lamp showed: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the reference solution.

Example 5

The identification method of the sertaconazole nitrate cream comprises the following steps: the method comprises the following steps:

(1) preparing a test solution: respectively taking 20mg of each of 10 groups of sertaconazole nitrate cream samples, adding 20ml of absolute ethyl alcohol, heating and dissolving in a water bath at 60 ℃, cooling, centrifuging at 2500r/min for 4min, taking supernate, adding the absolute ethyl alcohol with the same volume again, mixing, performing ultrasonic treatment for 15min, and filtering to obtain a sample solution;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the solution to prepare a sertaconazole nitrate solution with the mass concentration of 1mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a negative sample control solution: taking 20mg of cream auxiliary material which does not contain sertaconazole nitrate, and preparing a negative sample control solution according to the preparation method of the test solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and a concentrated ammonia solution according to a mass ratio of 50:50:20:2 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: mixing acetone 65:25:10 to obtain a developing solvent 2;

(4) chromatographic conditions and operation: according to thin layer chromatography, sucking 1 μ l each of the sample solution, the control solution and the sexual sample control solution, and spotting on the same silica gel GF₂₅₄Sequentially placing the thin-layer plate in a developing agent 1 at 110 ℃ for 15min, placing the thin-layer plate in a developing agent 2 at 60-80 ℃ for 9min, taking out, drying the thin-layer plate by using hot air at 60 ℃, immediately spraying an aluminum chloride solution with the mass concentration of 0.1% on the surface, continuously drying the thin-layer plate at 100 ℃, and inspecting the thin-layer plate under an ultraviolet lamp 254 nm; the results show that: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the reference solution, and the negative sample has no interference.

Example 6

The identification method of the sertaconazole nitrate cream comprises the following steps: the method comprises the following steps:

(1) preparing a test solution: respectively taking 20mg of each of 10 groups of sertaconazole nitrate cream samples, adding 20ml of absolute ethyl alcohol, heating and dissolving in a water bath at 60 ℃, cooling, centrifuging at 2500r/min for 4min, taking supernate, adding the absolute ethyl alcohol with the same volume again, mixing, performing ultrasonic treatment for 15min, and filtering to obtain a sample solution;

(2) preparing a reference solution: taking a sertaconazole nitrate reference substance, adding absolute ethyl alcohol to dissolve the sertaconazole nitrate reference substance, and diluting the solution to prepare a sertaconazole nitrate solution with the mass concentration of 1mg/ml, wherein the sertaconazole nitrate solution is used as a reference substance solution;

(3) preparing a negative sample control solution: taking 20mg of cream auxiliary material which does not contain sertaconazole nitrate, and preparing a negative sample control solution according to the preparation method of the test solution;

(3) preparing a developing agent: mixing trichloromethane, n-hexane, methanol and a concentrated ammonia solution according to a mass ratio of 50:50:20:2 to obtain a developing agent 1; adopting n-octanol and ethyl acetate: mixing acetone 65:25:10 to obtain a developing solvent 2;

(4) chromatographic conditions and operation: according to thin layer chromatography, sucking 1 μ l each of the sample solution, the control solution and the sexual sample control solution, and spotting on the same silica gel GF₂₅₄Sequentially placing the thin-layer plate in a developing agent 1 at 110 ℃ for 15min, placing the thin-layer plate in a developing agent 2 at 60-80 ℃ for 6min, taking out, drying the thin-layer plate by using hot air at 80 ℃, immediately spraying an aluminum chloride solution with the mass concentration of 0.5% on the surface, continuously drying the thin-layer plate at 100 ℃, and inspecting the thin-layer plate under an ultraviolet lamp 254 nm; the results show that: the position and color of the main spot displayed by the test solution are the same as those of the main spot displayed by the reference solution, and the negative sample has no interference.

Comparative example 1

The difference between the comparative example and the sertaconazole nitrate cream identification method of example 6 is that: the development was carried out with the developer 1 alone. The method specifically comprises the following steps: in step 4, according to thin layer chromatography, 1 μ l of each of the sample solution, the control solution and the sex sample control solution is spotted on the same silica gel GF₂₅₄Placing the thin-layer plate in a developing agent 1 at 110 deg.C for 21min, taking out, drying with 80 deg.C hot air, spraying 0.5% aluminum chloride solution on the surface, drying at 100 deg.C, and inspecting under 254nm ultraviolet lamp to obtain the main spots of the sample solution and the reference solution, wherein the main spots have the colors shown in the following table.

Comparative example 2

The difference between the comparative example and the sertaconazole nitrate cream identification method of example 6 is that: the developing agent 2 is prepared from 25:75 mass ratio of ethyl acetate: mixing with ethanol.

The results of the inspection at 254nm of an ultraviolet lamp show the position and color of the main spots of the test solution and the control solution as shown in the following table.

Comparative example 3

The difference between the comparative example and the sertaconazole nitrate cream identification method of example 6 is that: the developing agent 2 is prepared from n-octanol and ethyl acetate in a mass ratio of 70:25: 10: and acetone.

The results of the inspection at 254nm of an ultraviolet lamp show the position and color of the main spots of the test solution and the control solution as shown in the following table.

Example 7

This example differs from the sertaconazole nitrate cream identification method of example 6 in that: in step 4, silica gel GF₂₅₄And sequentially placing the thin-layer plate in a developing agent 1 at 110 ℃ for 10min, placing the thin-layer plate in a developing agent 2 at 60-80 ℃ for 6min, taking out, drying the thin-layer plate by using hot air at 80 ℃, immediately spraying an aluminum chloride solution with the mass concentration of 0.5% on the surface of the thin-layer plate, continuously drying the thin-layer plate at 100 ℃ until spots are clear, placing the thin-layer plate under an ultraviolet lamp at 254nm for inspection, and displaying the positions and colors of the main spots displayed by the test solution and the reference solution according to the results as shown in the following table.

The results of the sertaconazole nitrate cream identifications of the above examples and comparative examples show that the statistics are as follows:

as can be seen from the above table, repeated experiments show that the positions and colors of the main spots displayed by the test sample are the same as those of the main spots of the reference solution, the Rf value is moderate (generally, the Rf value is moderate from 0.5 to 0.8), the separation degree is good, no tailing exists, and the silica gel GF can be shortened₂₅₄The activation time of the thin-layer plate in the developing agent is below 30min, the thin-layer plate has good repeatability and stability, meanwhile, in the embodiments 5-6, the synchronous identification of the negative sample control solution is added, the result shows that no main spot appears in the negative sample, and no negative interference exists.

While example 7 further shortens the silica gel GF₂₅₄The thin layer plate has activation time in the developing agent, but has the phenomena of too small Rf value, reduced separation degree and partial tailing. Indicating control of silica gel GF₂₅₄The activation time of the thin-layer plate is as followsIs favorable for ensuring and improving the identification stability.

Compared with the comparative examples 1-3, the Rf value in the comparative example 1 is too small and the spots are fuzzy, which shows that the good separation degree can not be achieved within 30min, and the invention shows that the invention adopts the combination of the developing agent 1 and the developing agent 2 and reasonably controls the proportion relation, compared with the single developing agent 1, the activation time can be shortened, the separation is stable and the tailing is avoided, and the specific shift value Rf is effectively controlled. In example 2, the Rf value was comparable to that of example 6, but the spots were unclear, the degree of separation was poor, and streaking occurred; the Rf value in the comparative example 3 is overlarge and obvious trailing phenomenon appears, which shows that the invention is favorable for ensuring the spreading effect of the main spot and controlling good Rf value by controlling and adding a certain proportion of n-octanol, ethyl acetate and acetone to compound in the spreading agent, and the invention has stable separation and no trailing

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.