CN114487251B

CN114487251B - Thin-layer chromatography detection method for agilawood Shu Yupian

Info

Publication number: CN114487251B
Application number: CN202111457124.9A
Authority: CN
Inventors: 周建宇; 吴潇; 张红茹; 高广瑞; 韩志峰; 窦克娇; 盛娜
Original assignee: Jinyao Darentang Group Co ltd Longshunrong Pharmaceutical Factory
Current assignee: Jinyao Darentang Group Co ltd Longshunrong Pharmaceutical Factory
Priority date: 2021-12-02
Filing date: 2021-12-02
Publication date: 2023-11-03
Anticipated expiration: 2041-12-02
Also published as: CN114487251A

Abstract

The invention provides a thin-layer chromatography detection method for agilawood Yu Pian, and relates to the technical field of identification and detection of traditional Chinese medicine preparations. The detection method comprises the steps of firstly preprocessing agilawood Shu Yupian to obtain a sample solution of an agilawood depression relieving tablet; then respectively preprocessing the control medicinal materials of agilawood, magnolia officinalis, turmeric and glycyrrhizin to prepare a control solution; and then carrying out thin-layer identification analysis on the agilawood, magnolia officinalis, turmeric and glycyrrhizin in the agilawood Shu Yupian by using the agilawood depression relieving tablet sample solution and the control solution. The method makes the identification of the agilawood Shu Yupian more perfect by carrying out thin-layer identification analysis on the agilawood, the mangnolia officinalis, the curcuma longa and the glycyrrhizin in the agilawood Shu Yupian respectively, has the advantages of simplicity in operation, low toxicity and accuracy in identification, and is an effective and reliable quality detection method for the agilawood depression relieving tablet.

Description

Thin-layer chromatography detection method for agilawood Shu Yupian

Technical Field

The invention relates to the technical field of identification and detection of traditional Chinese medicine preparations, in particular to a thin-layer chromatography detection method of agilawood Yu Pian.

Background

The Chinese eaglewood tablet has the effects of removing blood stasis, relieving pain, soothing qi and stimulating appetite, and has good curative effects on symptoms such as depression, stomach pain, inappetence, dyspepsia, chest and abdominal distention, acid regurgitation and the like. However, the thin layer identification method for the agilawood Shu Yupian in the prior art has the defects of repeated identification components and content measurement.

Therefore, research and development of a thin layer identification method of agilawood Shu Yupian with simple operation, low toxicity and accurate identification are technical problems which are urgently needed to be solved in the field at present.

In view of this, the present invention has been made.

Disclosure of Invention

The invention aims to provide a thin-layer chromatography detection method for agilawood Yu Pian, which is characterized in that the thin-layer identification analysis is carried out on agilawood, magnolia officinalis, turmeric and glycyrrhizin in agilawood Shu Yupian respectively, so that the identification of agilawood Shu Yupian is more perfect, and the method has the advantages of simplicity in operation, low toxicity and accuracy in identification.

In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:

the invention provides a thin-layer chromatography detection method of agilawood Yu Pian, which comprises the following steps of:

preprocessing agilawood Shu Yupian to obtain a sample solution of the agilawood depression relieving tablet; then respectively preprocessing the control medicinal materials of agilawood, magnolia officinalis, turmeric and glycyrrhizin to prepare a control solution; and then carrying out thin-layer identification analysis on the agilawood, magnolia officinalis, turmeric and glycyrrhizin in the agilawood Shu Yupian by using the agilawood depression relieving tablet sample solution and the control solution.

Further, the control medicinal materials of the agilawood comprise agilawood;

Preferably, the control medicinal materials of magnolia officinalis comprise magnolol, honokiol and magnolia officinalis;

preferably, the control medicinal materials of turmeric comprise turmeric and curcumin;

further, the pretreatment method comprises any one of ultrasonic treatment, reflux treatment, dipping treatment or decoction treatment.

Further, when performing thin layer identification analysis on agilawood, a volume ratio of 10:1 as a developing agent; for inspection, the developed thin-layer plate was dried and then inspected under 254nm ultraviolet light.

Further, when performing thin-layer differential analysis on magnolia officinalis, a volume ratio of 10:4 as a developing agent; in the inspection process, the unfolded thin layer plate is dried, sprayed with sulfuric acid ethanol solution containing vanillin for color development, and then is inspected in sunlight;

further, the vanillin-containing sulfuric acid ethanol solution consists of vanillin and sulfuric acid ethanol with the concentration of 10%, and the vanillin-containing sulfuric acid ethanol solution comprises 1% of vanillin by mass.

Further, when thin layer differential analysis was performed on turmeric, a volume ratio of 16:0.8:0.1 trichloromethane-methanol-formic acid as developing agent.

Further, when liquiritin is subjected to thin layer identification analysis, the volume ratio is 15:1:1:2 ethyl acetate-formic acid-glacial acetic acid-water as developing agent; in the inspection, sulfuric acid ethanol solution is sprayed for color development, and then the color development is carried out under an ultraviolet lamp with the wavelength of 366nm for inspection.

Still further, the concentration of the sulfuric acid ethanol solution is 10wt%.

Further, the thin layer chromatography detection method also comprises the steps of negative test and durability test investigation.

Compared with the prior art, the invention has the beneficial effects that:

the invention provides a thin-layer chromatography detection method of agilawood Shu Yupian, which comprises the steps of firstly preprocessing agilawood Shu Yupian to obtain a sample solution of agilawood depression relieving tablets; then respectively preprocessing the control medicinal materials of agilawood, magnolia officinalis, turmeric and glycyrrhizin to prepare a control solution; and then carrying out thin-layer identification analysis on the agilawood, magnolia officinalis, turmeric and glycyrrhizin in the agilawood Shu Yupian by using the agilawood depression relieving tablet sample solution and the control solution. The method makes the identification of the agilawood Shu Yupian more perfect by carrying out thin-layer identification analysis on the agilawood, the mangnolia officinalis, the curcuma longa and the glycyrrhizin in the agilawood Shu Yupian respectively, has the advantages of simplicity in operation, low toxicity and accuracy in identification, and is an effective and reliable quality detection method for the agilawood depression relieving tablet.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.

FIG. 1 is a thin layer chromatography of eaglewood Shu Yupian provided in example 1 of the present invention;

FIG. 2 is a thin-layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian provided in example 1 of the present invention;

FIG. 3 is a thin-layer identification chromatogram of turmeric in eaglewood Shu Yupian provided in example 1 of the present invention;

FIG. 4 is a thin-layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian according to example 1 of the present invention;

FIG. 5 is a thin layer chromatography of the identification of eaglewood in eaglewood Shu Yupian at different temperatures according to example 2 of the present invention;

FIG. 6 is a thin layer chromatography of the identification of eaglewood in eaglewood Shu Yupian with different humidity according to example 2 of the present invention;

FIG. 7 is a thin-layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian at different temperatures provided in example 3 of the present invention;

FIG. 8 is a thin-layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian under different humidity conditions provided in example 3 of the present invention;

FIG. 9 is a thin layer chromatography of identification of turmeric in eaglewood Shu Yupian at different temperatures provided in example 4 of the present invention;

FIG. 10 is a thin layer chromatography of identification of turmeric in eaglewood Shu Yupian with different humidity as provided in example 4 of the present invention;

FIG. 11 is a thin-layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at different temperatures according to example 5 of the present invention;

fig. 12 is a thin-layer identification chromatogram of glycyrrhizin in eaglewood Shu Yupian under different humidity conditions provided in example 5 of the present invention.

Detailed Description

The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

According to one aspect of the invention, a thin layer chromatography detection method of agilawood Yu Pian comprises the following steps:

The invention provides a thin-layer chromatography detection method of agilawood Shu Yupian, which comprises the steps of firstly preprocessing agilawood Shu Yupian to obtain a sample solution of agilawood depression relieving tablets; then respectively preprocessing the control medicinal materials of agilawood, magnolia officinalis, turmeric and glycyrrhizin to prepare a control solution; and then carrying out thin-layer identification analysis on the agilawood, magnolia officinalis, turmeric and glycyrrhizin in the agilawood Shu Yupian by using the agilawood depression relieving tablet sample solution and the control solution. The method makes the identification of the agilawood Shu Yupian more perfect by carrying out thin-layer identification analysis on the agilawood, the magnolia officinalis, the turmeric and the glycyrrhizin in the agilawood Shu Yupian respectively, and has the advantages of simplicity in operation, low toxicity and accuracy in identification.

In a preferred embodiment of the present invention, the control medicinal material of the agilawood comprises agilawood;

in a preferred embodiment of the present invention, the control medicinal material of magnolia officinalis comprises magnolol, honokiol and magnolia officinalis;

in a preferred embodiment of the present invention, the control drug of turmeric comprises turmeric and curcumin.

In a preferred embodiment of the present invention, the method of pretreatment comprises any one of sonication, reflux, maceration or decoction.

In a preferred embodiment of the present invention, when performing thin layer differential analysis on agilawood, a volume ratio of 10:1 as a developing agent; for inspection, the developed thin-layer plate was dried and then inspected under 254nm ultraviolet light.

Preferably, the thin layer identification analysis method of the agilawood in the agilawood Shu Yupian comprises the following steps:

(a1) Adding 1g of a sample of the agalloch eaglewood Shu Yu Pian into 30ml of petroleum ether, carrying out ultrasonic treatment for 30min, filtering to obtain a filtrate, and then dissolving residues obtained by evaporating the filtrate into 2ml of methanol to obtain a sample solution A of the agalloch eaglewood Shu tablet;

(b1) Taking 0.3g of agilawood as a reference substance, adding 30ml of methanol, carrying out ultrasonic treatment for 30min, filtering, and concentrating the filtrate under reduced pressure until the filtrate is dried; then adding petroleum ether 10ml, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding methanol 1ml into residues for dissolution to obtain agilawood reference substance solution;

(c1) Taking 2 μl of agilawood depression relieving tablet test solution A and 1 μl of agilawood reference substance solution, respectively spotting on the same silica gel G thin layer plate, wherein the volume ratio is 10:1, developing with dichloromethane-ethyl acetate as developing agent, taking out, air drying, and inspecting under 254nm ultraviolet light.

In a preferred embodiment of the present invention, when performing thin layer differential analysis on magnolia bark, a volume ratio of 10:4 as a developing agent; in the inspection process, the unfolded thin layer plate is dried, sprayed with sulfuric acid ethanol solution containing vanillin for color development, and then is inspected in sunlight;

Preferably, the thin layer differential analysis method of magnolia officinalis in agilawood Shu Yupian comprises the following steps:

(a2) Adding 1g of a sample of the agalloch eaglewood Shu Yu Pian into 40ml of ethyl acetate, carrying out ultrasonic treatment for 30min, filtering to obtain a filtrate, and then dissolving residues obtained by evaporating the filtrate into 1ml of methanol to obtain a sample solution B of the agalloch eaglewood Shu tablet;

(b2) Adding 0.2g of magnolia officinalis into 20ml of ethyl acetate, performing ultrasonic treatment for 30min, filtering, evaporating filtrate to dryness, and dissolving residues in 1ml of methanol to obtain a magnolia officinalis reference medicinal material solution;

adding 1mg of magnolol into 1ml of methanol to prepare a magnolol control solution;

adding honokiol 1mg into 1ml of methanol to obtain honokiol control solution;

(c2) Taking 2 mu l of each of a sample solution B of the agilawood depression relieving tablet, a magnolia officinalis control medicinal material solution, a magnolol control solution and a honokiol control solution, respectively and putting the sample solution B, the magnolol control solution, the honokiol control solution and the honokiol control solution on the same silica gel G thin layer plate, wherein the volume ratio is 10:4 as a developing agent; in the inspection, the developed thin layer plate is dried, sprayed with a sulfuric acid ethanol solution containing vanillin for color development, and then is inspected in sunlight.

In the above preferred embodiment, the vanillin-containing sulfuric acid ethanol solution consists of vanillin and sulfuric acid ethanol with a concentration of 10%, and the vanillin-containing sulfuric acid ethanol solution has a mass percentage of vanillin of 1%.

In a preferred embodiment of the present invention, when performing thin layer differential analysis of turmeric, a volume ratio of 16:0.8:0.1 trichloromethane-methanol-formic acid as developing agent.

Preferably, the thin layer identification analysis method of turmeric in agilawood Shu Yupian comprises the following steps:

(a3) Adding 2g of a sample of the agalloch eaglewood Shu Yu Pian into 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 30min, filtering to obtain a filtrate, and then dissolving residues obtained by evaporating the filtrate into 2ml of methanol to obtain an agalloch eaglewood Shu tablet sample solution C;

(b3) Adding 0.2g of turmeric into 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 30min, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues for dissolution to obtain turmeric reference medicinal material solution;

adding 0.5mg of curcumin into 1ml of methanol to prepare curcumin control solution;

(c3) Taking 1 μl of each of the agilawood depression relieving tablet test solution C, the turmeric reference medicinal material solution and the curcumin reference solution, respectively putting the sample solution C, the turmeric reference medicinal material solution and the curcumin reference solution on the same silica gel G thin layer plate, and adopting the volume ratio of 16:0.8:0.1 trichloromethane-methanol-formic acid as developing agent; in the inspection, the unfolded thin layer plate is dried and then is inspected in sunlight.

In a preferred embodiment of the present invention, when liquiritin is subjected to thin layer differential analysis, a volume ratio of 15:1:1:2 ethyl acetate-formic acid-glacial acetic acid-water as developing agent; in the inspection, sulfuric acid ethanol solution is sprayed for color development, and then the color development is carried out under an ultraviolet lamp with the wavelength of 366nm for inspection.

In the above preferred embodiment, the concentration of the sulfuric acid ethanol solution is 10wt%.

Preferably, the thin layer identification analysis method of glycyrrhizin in agilawood Shu Yupian comprises the following steps:

(a4) Adding 5g of a agalloch eaglewood Yu Pian sample into 40ml of water, carrying out ultrasonic treatment for 30min, centrifuging, filtering to obtain a filtrate, extracting the filtrate with 30ml of ethyl acetate for 2 times, combining ethyl acetate solutions, recovering the solvent under reduced pressure until the solvent is dry, and dissolving the residue in 1ml of methanol to obtain an agalloch eaglewood depression relieving tablet sample solution D;

(b4) Adding 1mg of liquiritin into 1ml of methanol to obtain a liquiritin control solution;

(c4) Taking 3 μl of a sample solution D of the agilawood depression relieving tablet and 2 μl of a glycyrrhizin control solution, respectively, and respectively spotting on the same silica gel G thin layer plate, wherein the volume ratio is 15:1:1:2 ethyl acetate-formic acid-glacial acetic acid-water as developing agent; in the process of inspection, spraying sulfuric acid ethanol solution for color development, and then placing under an ultraviolet lamp with the wavelength of 366nm for inspection;

in a preferred embodiment of the present application, the thin layer chromatography detection method further comprises the steps of a negative test and a durability test investigation.

The technical scheme of the application will be further described with reference to examples.

Note that: the samples in the examples of the present application were selected as follows:

Agalloch eaglewood Shu Yupian, lot numbers 400009, 400010, FJ40007, FJ40008, GA40009, GA40010, FF40004, provided by Dai-shun banyan pharmaceutical factory, new pharmaceutical group Co., tianjin;

agilawood control medicinal material, lot 121222-201203, chinese food and drug verification institute;

magnolia officinalis control medicinal material, lot number 121285-201303, chinese food and drug verification institute;

turmeric reference medicinal material, lot 121188-201605, national food and drug verification institute;

costunolide, lot number 111524-201911, national food and drug verification institute;

dehydrocostuslactone, lot 111525-201912, national food and drug verification institute;

magnolol, batch No. 110729-201714, content 100.0%, chinese food and drug inspection institute;

honokiol, batch number 110730-201614, content 99.3%, national food and drug verification institute;

curcumin, lot 110823-201706, chinese food and drug verification institute;

glycyrrhizin, lot 111610-201908, national food and drug verification institute.

The instrumentation used was as follows:

KQ-400VDE ultrasonic instrument, kunshan, ultrosophy instruments Co., ltd;

MS105 electronic balance, mertler company;

AL204-IC electronic balance, metrehler company;

An explosion-proof refrigerator LIEBHERR MeDiLine;

thin layer chromatography imaging system, cab UVIS, germany DESAGA Technology;

(III) reagent drugs are as follows:

the methanol is chromatographic pure, absolute ethanol, dichloromethane, chloroform, acetone, cyclohexane, petroleum ether (60-90 ℃), ethyl acetate, formic acid, glacial acetic acid, sulfuric acid, vanillin, and the water is purified water.

Thin layer chromatography silica gel prefabricated plate, model HSG, lot numbers 20181212 and 20200701, institute of chemical industry in tabacco market;

example 1

(one), thin layer identification analysis of agilawood in agilawood Shu Yupian:

(1) Taking agalloch eaglewood Yu Pian (batch No. 400009, FJ40007, GA 40009), pulverizing into fine powder, taking about 1g, adding 30ml petroleum ether (60-90 deg.C), ultrasonic treating for 30 min, filtering, evaporating filtrate, and dissolving residue with 2ml methanol to obtain sample solution.

(2) Grinding lignum Aquilariae Resinatum negative sample particles into fine powder, adding 30ml of petroleum ether (60-90deg.C) to about 1g of the powder, and preparing into lignum Aquilariae Resinatum negative sample solution by the same method as sample solution.

(3) Taking 0.3g of agilawood reference medicine, adding 30ml of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, concentrating the filtrate under reduced pressure (water bath 50 ℃) until the filtrate is dry, adding 10ml of petroleum ether (60-90 ℃) and carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain the agilawood reference medicine solution.

(4) 2 μl of agilawood control medicinal material solution and 1 μl of agilawood negative sample solution (batch No. 400009, FJ40007, GA 40009) are respectively absorbed, 1 μl of agilawood negative sample solution and 1 μl of agilawood negative sample solution are respectively spotted on the same high-efficiency silica gel G thin layer plate (smoke table HSG,110 ℃ for 30 minutes), dichloromethane-ethyl acetate (10:1) solution is taken as a developing agent (a developing cylinder is pre-balanced for 20 min), and the mixture is developed, taken out and dried, and is placed under ultraviolet light (254 nm) for detection.

The specific detection result is shown in fig. 1, where fig. 1 is a thin-layer identification chromatogram of eaglewood in eaglewood Shu Yupian in this embodiment. Wherein, lane1 is agilawood control medicinal material solution; lane2 is a sample solution of lignum Aquilariae Resinatum tablet (lot number: 400009); lane3 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane4 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane5 is a agilawood negative sample solution.

As can be seen from FIG. 1, in each sample chromatogram of this example, 3 fluorescence spots of the same color were displayed at the positions corresponding to the control chromatogram, and the negative positions were not interfered, so that the spot separation was good.

(II), thin-layer identification analysis of magnolia officinalis in agilawood Shu Yupian:

(1) Taking appropriate amount of lignum Aquilariae Resinatum Yu Pian (batch No. 400009, FJ40007, and GA 40009), pulverizing into fine powder, adding ethyl acetate 40ml about 1g, ultrasonic treating for 30 min, filtering, evaporating filtrate, and dissolving residue with methanol 1ml to obtain sample solution.

(2) Taking a proper amount of magnolia bark negative sample particles, grinding into fine powder, taking about 1g, adding 40ml of ethyl acetate, and preparing the magnolia bark negative sample solution by the same test sample solution preparation method.

(3) Taking a proper amount of magnolol reference substance, adding methanol to prepare a magnolol reference substance solution containing 1mg of magnolol per 1 ml.

Taking a proper amount of honokiol reference substance, adding methanol to prepare a honokiol reference substance solution containing 1mg per 1 ml.

Taking 0.2g of magnolia officinalis control medicinal material, adding 20ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a magnolia officinalis control medicinal material solution.

(4) Respectively sucking 2 μl of magnolol control solution and 2 μl of magnolol control solution, 2 μl of control medicinal solution, 2 μl of agilawood depression relieving tablet sample solution (batch No. 400009, FJ40007, GA 40009), 2 μl of magnolol negative sample solution, spotting in strip form on the same high-efficiency silica gel G thin layer plate (smoke table HSG,110 ℃ for 30 min), taking cyclohexane-acetone (10:4) solution as developing agent (pre-balancing for 20min in a developing cylinder), developing, taking out, air drying, spraying 1% vanillin 10% sulfuric acid ethanol solution, heating until spots are clear, and inspecting in sunlight.

The specific detection result is shown in fig. 2, where fig. 2 is a thin-layer identification chromatogram of magnolia officinalis in agilawood Shu Yupian in this embodiment. Wherein, lane1 is magnolol reference substance solution; lane2 is honokiol reference substance solution; lane3 is a magnolia officinalis control medicinal material solution; lane4 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane5 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane6 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane7 is a magnolia negative sample solution.

As can be seen from FIG. 2, in each sample chromatogram of this example, spots of the same color are present at the positions corresponding to the corresponding positions of the magnolia bark control and the control chromatogram, no interference is present at the negative corresponding positions, and the separation degree of each spot is good.

(III), thin-layer identification analysis of turmeric in agilawood Shu Yupian:

(1) Taking appropriate amount of lignum Aquilariae Resinatum Yu Pian (batch number: FJ40007, FJ40008, and GA 40009), grinding into fine powder, adding 20ml of absolute ethanol into about 2g, ultrasonic treating for 30 min, filtering, evaporating filtrate, and dissolving residue with 2ml of methanol to obtain sample solution.

(2) Grinding appropriate amount of Curcuma rhizome negative sample particles into fine powder, adding 20ml of absolute ethanol into about 2g, and preparing Curcuma rhizome negative sample solution by the same method as the sample solution preparation method.

(3) Taking a proper amount of curcumin reference substance, adding methanol to prepare a curcumin reference substance solution containing 0.5mg per 1 ml.

Taking turmeric reference medicinal material 0.2g, adding absolute ethanol 20ml, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding methanol 1ml into residues to dissolve the residues to obtain reference medicinal material solution.

(4) Respectively sucking 1 μl of curcumin control solution, 1 μl of control medicinal solution, 1 μl of agilawood Shu Yupian (lot number: FJ40007, FJ40008, GA 40009) sample solution and 1 μl of turmeric negative sample solution, spotting in strip shape on the same high-efficiency silica gel G thin layer plate (smoke table HSG,110 ℃ for 30 min), taking chloroform-methanol-formic acid (16:0.8:0.1) solution as developing agent (developing cylinder solvent vapor pre-balance for 20 min), developing, taking out, air drying, and inspecting under sunlight.

The specific detection results are shown in fig. 3, where fig. 3 is a thin-layer identification chromatogram of turmeric in agilawood Shu Yupian of this embodiment. Wherein Lane1 is curcumin reference solution; lane2 is turmeric reference medicinal material solution; lane3 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane4 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane5 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane6 is a turmeric negative sample solution.

As can be seen from fig. 3, in each chromatogram of the sample in this embodiment, spots of the same color are located at the positions corresponding to the chromatograms of the turmeric reference and the reference medicinal materials, no interference is generated at the negative positions, the spot separation degree is good, and the specificity of the method is good.

(IV), thin-layer identification analysis of glycyrrhizin in agilawood Shu Yupian:

(1) Taking appropriate amount of lignum Aquilariae Resinatum Yu Pian (batch No. 400009, FJ40007, GA 40009), grinding into fine powder, taking about 5.0g, adding 40ml of water, ultrasonic treating for 30 min, centrifuging (3180 rpm,15 min), collecting supernatant, filtering, shaking and extracting filtrate with ethyl acetate for 2 times, each time for 30ml, mixing ethyl acetate solutions, recovering solvent at 50deg.C under reduced pressure to dryness, and dissolving residue with 1ml of methanol to obtain test solution.

(2) Grinding appropriate amount of glycyrrhizin negative sample particles into fine powder, taking about 5.0g, adding water 40ml, and preparing into glycyrrhizin negative sample solution by the same test sample solution preparation method.

(3) Adding methanol into appropriate amount of glycyrrhizin reference substance to obtain 1mg of glycyrrhizin reference substance solution per 1 ml.

(4) Respectively sucking 2 μl of control solution, 3 μl of each of the sample solutions of lignum Aquilariae Resinatum Shu Yupian (batch No. 400009, FJ40007, GA 40009) and 3 μl of glycyrrhizin negative sample solution, spotting in strip form on the same high-efficiency silica gel G thin layer plate (yellow sea HSG,110 deg.C for 30 min), taking ethyl acetate-formic acid-glacial acetic acid-water (15:1:1:2) solution as developing agent (developing cylinder solvent vapor pre-balancing for 20 min), developing, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating until the color of spots is clear, and placing under ultraviolet light (366 nm) for inspection.

The specific detection result is shown in fig. 4, and fig. 4 is a thin-layer identification chromatogram of glycyrrhizin in agilawood Shu Yupian according to the embodiment. Wherein Lane1 is a control solution of liquiritin; lane2 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane3 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane4 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane5 is a glycyrrhizin negative sample solution.

As can be seen from FIG. 4, in each sample chromatogram of this example, there was fluorescence spots of the same color at the positions corresponding to those of the glycyrrhizin control chromatogram, and the negative positions were not interfered, and the spot separation degree was good, and the method was excellent in specificity.

As can be seen from fig. 1 to 4, in the chromatograms of the samples in this example, fluorescent spots of the same color were formed at positions corresponding to the chromatograms of the reference substances of eaglewood, magnolia officinalis, turmeric and glycyrrhizin, and the negative positions were not interfered, and the spot separation degree and the specificity were good. This means that the test article is a good product.

Example 2 durability investigation of agilawood in thin layer discrimination analysis of agilawood:

(one), temperature investigation:

(4) 2 μl of agilawood control medicinal material solution is respectively absorbed, 2 μl of agilawood depression relieving tablet sample solution (batch number: 400009, FJ40007, GA 40009) and 2 μl of agilawood negative sample solution are respectively spotted on the same high-efficiency silica gel G thin layer plate (smoke table HSG, all 110 ℃ for 30 minutes), methylene dichloride-ethyl acetate (10:1) solution is taken as a developing agent (a developing cylinder is pre-balanced for 20 minutes), and the solution is developed, taken out and dried respectively at 4 ℃ (refrigerator) and 24 ℃ (room temperature) and is placed under ultraviolet light (254 nm) for detection.

The specific shift values of the components of this example at different temperatures are shown in the following table:

note that: the above data are the average of the different batches of spots

The specific detection results are shown in fig. 5, where fig. 5 is a thin layer identification chromatogram of agilawood in agilawood Shu Yupian at different temperatures in the present embodiment.

FIG. 5 (a) shows a thin layer chromatography of the agilawood Shu Yupian at a temperature of 4 ℃;

FIG. 5 (b) shows a thin layer chromatography of the agilawood Shu Yupian at 24 ℃;

wherein, lane1 is agilawood control medicinal material solution; lane2 is a sample solution of lignum Aquilariae Resinatum tablet (lot number: 400009); lane3 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane4 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane5 is a agilawood negative sample solution.

As can be seen from FIG. 5, the spot ratio shift value increases with increasing temperature at 4℃and 24 ℃. In each chromatogram of the test sample, fluorescent spots with the same color are arranged at the positions corresponding to the chromatograms of the control medicinal materials, and the separation degree of each spot is good without interference at the negative position.

(II), humidity investigation:

(4) 2 μl of agilawood control medicinal material solution and 2 μl of agilawood depression relieving tablet sample solution (batch numbers: 400009, FJ40007 and GA 40009) and 2 μl of agilawood negative sample solution are respectively absorbed, respectively and strip-shaped sample is applied on the same high-efficiency silica gel G thin layer plate (smoke table HSG, all 110 ℃ for 30 minutes), the thin layer plates after sample application are respectively placed in a drier (containing sulfuric acid solutions with different concentrations) with relative humidity of 18%, 47%, 65%, 72% and 88% (about 1 hour), methylene dichloride-ethyl acetate (10:1) solution is used as a developing agent (a developing cylinder is pre-balanced for 20 minutes), and the thin layer plates are developed, taken out and dried at room temperature and are subjected to ultraviolet light (254 nm) for detection.

The specific shift values of the components of this example at different humidities are shown in the following table:

the specific detection results are shown in fig. 6, where fig. 6 is a thin-layer identification chromatogram of agilawood in agilawood Shu Yupian under different relative humidity in this embodiment.

FIG. 6 (a) shows a thin layer identification chromatogram of eaglewood in eaglewood Shu Yupian under 18% humidity;

FIG. 6 (b) shows a thin layer chromatography of eaglewood in eaglewood Shu Yupian with a humidity of 47%;

FIG. 6 (c) shows a thin layer chromatography of the eaglewood of eaglewood Shu Yupian with 65% humidity;

FIG. 6 (d) shows a thin layer identification chromatogram of eaglewood in eaglewood Shu Yupian at 72% humidity;

FIG. 6 (e) shows a thin layer identification chromatogram of lignum Aquilariae Resinatum in lignum Aquilariae Resinatum Shu Yupian at 88% humidity;

wherein 1 is agilawood control medicinal material solution; 2 is a sample solution of the lignum Aquilariae Resinatum tablet (batch number: 400009); 3 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); 4 is a sample solution of the lignum Aquilariae Resinatum tablet (batch number: GA 40009); 5 is a agilawood negative sample solution.

As can be seen from fig. 6, at 72% and 88% relative humidity, the top two spots may coincide with adjacent spots, with interference in the negative position; at relative humidity 18%, 47% and 65%, the individual spots were well separated and the negative position was undisturbed.

Example 3 durability investigation of magnolia officinalis in a thin layer differential analysis of eaglewood:

(one), temperature investigation:

(4) 2 mu l of magnolol control solution and 2 mu l of magnolol control solution are respectively sucked, 2 mu l of agilawood depression relieving tablet test solution (batch No. 400009, FJ40007 and GA 40009) are respectively sucked, 2 mu l of magnolol negative sample solution is respectively sucked, strip sample points are respectively placed on the same high-efficiency silica gel G thin layer plate (smoke table HSG and 110 ℃ for 30 minutes), cyclohexane-acetone (10:4) solution is used as a developing agent (a developing cylinder is pre-balanced for 20 minutes), and the mixture is respectively developed, taken out and dried in the air at 4 ℃ (refrigerator), 10 ℃ (refrigerator) and 24 ℃ (room temperature), and 10% sulfuric acid ethanol solution sprayed with 1% vanillin is heated until the spots are clear in color development, and is inspected in sunlight.

The specific shift values of the components at different temperatures in this example are shown in the following table:

the specific detection results are shown in fig. 7, where fig. 7 is a thin-layer identification chromatogram of magnolia officinalis in agilawood Shu Yupian at different temperatures in this embodiment.

FIG. 7 (a) shows a thin-layer identification chromatogram of Magnolia officinalis in Aquilaria sinensis Shu Yupian at 4deg.C;

FIG. 7 (b) shows a thin-layer identification chromatogram of Magnolia officinalis in Aquilaria sinensis Shu Yupian at 10deg.C;

FIG. 7 (c) shows a thin-layer identification chromatogram of Magnolia officinalis in Aquilaria sinensis Shu Yupian at 24deg.C;

wherein, lane1 is magnolol reference substance solution; lane2 is honokiol reference substance solution; lane3 is a magnolia officinalis control medicinal material solution; lane4 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane5 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane6 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane7 is a magnolia negative sample solution.

As can be seen from FIG. 7, under the low temperature condition of 4 ℃, honokiol is not separated from adjacent spots, and the negative position is interfered; the two main spots can be detected at 10 ℃ and 24 ℃ and have better separation degree, and the negative position is not interfered.

(II), humidity investigation:

(3) Taking a proper amount of magnolol reference substance, adding methanol to prepare a magnolol reference substance solution containing 1mg of magnolol per 1 ml. Taking a proper amount of honokiol reference substance, adding methanol to prepare a honokiol reference substance solution containing 1mg per 1 ml. Taking 0.2g of magnolia officinalis control medicinal material, adding 20ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a magnolia officinalis control medicinal material solution.

(4) 2 mu l of magnolol control solution and 2 mu l of magnolol control solution are respectively sucked, 2 mu l of agilawood depression relieving tablet sample solution (batch No. 400009, FJ40007 and GA 40009) are respectively sucked, 2 mu l of magnolol negative sample solution is respectively sucked, strip sample application is carried out on the same high-efficiency silica gel G thin layer plate (smoke table HSG and activation is carried out at 110 ℃ for 30 minutes), the thin layer plates after sample application are respectively placed in a drier (containing sulfuric acid solutions with different concentrations) with relative humidity of 18%, 47%, 72% and 88% (about 1 hour), cyclohexane-acetone (10:4) solution is taken as a developing agent (developing cylinder is pre-balanced for 20 minutes), developed, taken out and dried, and 10% sulfuric acid ethanol solution sprayed with 1% vanillin is heated until the spots are clear in sunlight.

The specific shift values of the components under different humidity conditions in this example are shown in the following table:

the specific detection results are shown in fig. 8, where fig. 8 is a thin-layer identification chromatogram of magnolia officinalis in agilawood Shu Yupian under different humidity in this embodiment.

FIG. 8 (a) shows a thin layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian with a humidity of 18%;

FIG. 8 (b) shows a thin-layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian with a humidity of 47%;

FIG. 8 (c) shows a thin layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian at 72% humidity;

FIG. 8 (d) shows a thin layer identification chromatogram of Magnolia officinalis in eaglewood Shu Yupian with 88% humidity;

As can be seen from FIG. 8, under the condition of the relative humidity of 88%, the honokiol spots are not well separated from the adjacent spots and coincide with the spots, so that the negative positions are disturbed; under the conditions of 18%, 47% and 72% relative humidity, the separation degree of each spot is good, and the negative position is not interfered.

Example 4 durability investigation of turmeric in a thin layer differential analysis of eaglewood:

(one), temperature investigation:

(3) Taking a proper amount of curcumin reference substance, adding methanol to prepare a curcumin reference substance solution containing 0.5mg per 1 ml. Taking turmeric reference medicinal material 0.2g, adding absolute ethanol 20ml, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding methanol 1ml into residues to dissolve the residues to obtain reference medicinal material solution.

(4) Respectively sucking 1 μl of control solution, 2 μl of lignum Aquilariae Resinatum Shu Yupian (batch number: FJ40007, FJ40008, GA 40009) and 2 μl of Curcuma rhizome negative sample solution, spotting in strip shape on the same high efficiency silica gel G thin layer plate (smoke stage HSG, 110deg.C for 30 min), taking chloroform-methanol-formic acid (16:0.8:0.1) solution as developing agent (developing cylinder solvent vapor pre-balancing for 20 min), developing at 4deg.C and 25deg.C (refrigerator), taking out, air drying, and inspecting under sunlight.

the specific detection results are shown in fig. 9, where fig. 9 is a thin-layer identification chromatogram of turmeric in agilawood Shu Yupian at different temperatures in the present embodiment.

FIG. 9 (a) shows a thin-layer identification chromatogram of turmeric in eaglewood Shu Yupian at a temperature of 4 ℃;

FIG. 9 (b) shows a thin-layer identification chromatogram of turmeric in eaglewood Shu Yupian at 25deg.C;

wherein Lane1 is curcumin reference solution; lane2 is turmeric reference medicinal material solution; lane3 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane4 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane5 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane6 is a turmeric negative sample solution.

As is clear from FIG. 9, the specific shift value of spot 1 (curcumin) does not change much under the conditions of 4℃and 25℃and the specific shift value of spots 2 and 3 becomes small with the increase of temperature, and the degree of separation of each spot is good and the negative position is not disturbed.

(II), humidity investigation:

(2) Grinding appropriate amount of Curcuma rhizome negative sample particles into fine powder, taking about 2g, adding absolute ethanol 20ml, and preparing Curcuma rhizome negative sample solution by the same method as the sample solution preparation method.

(4) And respectively sucking 1 μl of the control solution, 2 μl of the sample solution of lignum Aquilariae Resinatum Shu Yupian (lot number: FJ40007, FJ40008, GA 40009) and 2 μl of the turmeric negative sample solution, applying the strip sample on the same high-efficiency silica gel G thin layer plate (smoke table HSG,110 ℃ for 30 min), placing the thin layer plate after sample application in a drier with relative humidity of 18%, 47% and 88% (containing sulfuric acid with different concentrations) (about 1 hr), taking chloroform-methanol-formic acid (16:0.8:0.1) solution as developing agent (developing cylinder solvent vapor pre-balancing for 20 min), developing at room temperature, taking out, air drying, and inspecting under sunlight.

the specific detection results are shown in fig. 10, and fig. 10 is a thin-layer identification chromatogram of turmeric in agilawood Shu Yupian under different humidity conditions in this embodiment.

FIG. 10 (a) shows a thin layer identification chromatogram of turmeric in lignum Aquilariae Resinatum Shu Yupian at 18% humidity;

FIG. 10 (b) shows a thin-layer identification chromatogram of turmeric in eaglewood Shu Yupian at 47% humidity;

FIG. 10 (c) shows a thin layer identification chromatogram of turmeric in lignum Aquilariae Resinatum Shu Yupian at 88% humidity;

As can be seen from FIG. 10, the specific shift value of the spot 1 (curcumin control) was not changed much under conditions of 18%, 47% and 88% humidity, the specific shift value of the spot 2 was small under conditions of 88% humidity, the specific shift value of the spot 3 was decreased with the increase of humidity, the degree of separation of each spot was good, and the negative position was not disturbed.

Example 5 durability investigation of glycyrrhizin in a thin layer differential analysis of eaglewood:

(one), temperature investigation:

(4) 2 μl of control solution and 3 μl of agilawood Shu Yupian (batch No. 400009, FJ40007, GA 40009) to be tested and 3 μl of glycyrrhizin negative sample solution are respectively sucked, the strip sample is spotted on the same high-efficiency silica gel G thin layer plate (yellow sea HSG,110 ℃ for 30 minutes), ethyl acetate-formic acid-glacial acetic acid-water (15:1:1:2) solution is taken as a developing agent (solvent vapor pre-balancing for 20 minutes), and the solution is developed, taken out and dried under the conditions of 4 ℃ (refrigerator) and 23 ℃ (room temperature) respectively, sprayed with 10% sulfuric acid ethanol solution, heated until the spots develop clearly, and detected under ultraviolet light (366 nm).

The ratio shift values of glycyrrhizin at different temperatures in this example:

the specific detection results are shown in fig. 11, where fig. 11 is a thin-layer identification chromatogram of glycyrrhizin in eaglewood Shu Yupian at different temperatures according to the present embodiment.

FIG. 11 (a) shows a thin-layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at 4deg.C;

FIG. 11 (b) shows a thin-layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at 23deg.C;

Wherein Lane1 is a control solution of liquiritin; lane2 is a sample solution of the lignum Aquilariae Resinatum depression relieving tablet (batch number: 400009); lane3 is a sample solution of the agilawood depression relieving tablet (batch number: FJ 40007); lane4 is a sample solution of lignum Aquilariae Resinatum tablet (batch number: GA 40009); lane5 is a glycyrrhizin negative sample solution.

As is clear from FIG. 11, the glycyrrhizin spot ratio shift value increases with increasing temperature at 4℃and 23 ℃. In each chromatogram of the sample, fluorescent spots with the same color are arranged at the positions corresponding to the chromatograms of the reference sample under ultraviolet light (366 nm), no interference exists at the negative positions, and the spot separation degree is good.

(II), humidity investigation:

(4) Respectively sucking 2 μl of control solution, 3 μl of agilawood Shu Yupian (batch No. 400009, FJ40007, GA 40009) to be tested solution and 3 μl of licorice negative sample solution, applying the sample on the same silica gel G thin layer plate (yellow sea HSG,110 ℃ for 30 min), respectively placing the thin layer plates after sample application in a drier with relative humidity of 18%, 47% and 88% (containing sulfuric acid solutions with different concentrations) (about 1 hr), taking ethyl acetate-formic acid-glacial acetic acid-water (15:1:1:2) solution as developing agent (developing cylinder solvent steam pre-balancing for 20 min), developing at room temperature, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating until the color of the spots is clear, and checking under ultraviolet light (366 nm).

The ratio shift value of glycyrrhizin under different humidity in this example:

the specific detection results are shown in fig. 12, and fig. 12 is a thin-layer identification chromatogram of glycyrrhizin in eaglewood Shu Yupian under different humidity in this embodiment.

FIG. 12 (a) shows a thin layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at 18% humidity;

FIG. 12 (b) shows a thin-layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at 47% humidity;

FIG. 12 (c) shows a thin layer identification chromatogram of glycyrrhizin in lignum Aquilariae Resinatum Shu Yupian at 88% humidity;

As is clear from FIG. 11, the glycyrrhizin spot ratio shift value increased with the increase of the humidity under the conditions of the humidity of 18%, 47% and 88%, respectively. In each chromatogram of the sample, fluorescent spots with the same color are arranged at the positions corresponding to the chromatograms of the reference sample under ultraviolet light (366 nm), no interference exists at the negative positions, and the spot separation degree is good.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims

1. A thin layer chromatography detection method of agilawood Yu Pian, which is characterized by comprising the following steps of: thin layer identification analysis of eaglewood in eaglewood Shu Yupian, thin layer identification analysis of officinal magnolia bark in eaglewood Shu Yupian, thin layer identification analysis of turmeric in eaglewood Shu Yupian and thin layer identification analysis of glycyrrhizin in eaglewood Shu Yupian;

the thin layer identification analysis of the agilawood in the agilawood Shu Yupian comprises the following steps:

pulverizing lignum Aquilariae Resinatum tablet, adding petroleum ether, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain sample solution; grinding lignum Aquilariae Resinatum negative sample particles into fine powder, adding petroleum ether into the powder, and preparing into lignum Aquilariae Resinatum negative sample solution with the sample solution preparation method; performing ultrasonic treatment on lignum Aquilariae Resinatum reference material with methanol, filtering, concentrating the filtrate under reduced pressure to dry, performing ultrasonic treatment with petroleum ether, filtering, evaporating the filtrate to dry, and dissolving the residue with methanol to obtain lignum Aquilariae Resinatum reference material solution;

respectively sucking a agilawood control medicinal material solution, a agilawood depression relieving tablet sample solution and a agilawood negative sample solution, and spotting the sample solution in a strip shape on the same high-efficiency silica gel G thin layer plate according to the volume ratio of 10:1, developing with dichloromethane-ethyl acetate as developing agent, taking out, air drying, and inspecting under ultraviolet light of 254 nm;

The thin-layer differential analysis of magnolia officinalis in agilawood Shu Yupian comprises the following steps:

pulverizing lignum Aquilariae Resinatum tablet into fine powder, adding ethyl acetate, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue in methanol to obtain sample solution; taking a proper amount of magnolia bark negative sample, grinding the magnolia bark negative sample into fine powder, and adding ethyl acetate into the mixture to prepare a magnolia bark negative sample solution by a sample solution preparation method; taking a proper amount of honokiol reference substance, adding methanol to prepare honokiol reference substance solution; taking a proper amount of magnolol reference substance, adding methanol to prepare a magnolol reference substance solution; adding ethyl acetate into cortex Magnolia officinalis control medicinal material, performing ultrasonic treatment, filtering, evaporating filtrate, and dissolving residue with methanol to obtain cortex Magnolia officinalis control medicinal material solution;

respectively sucking magnolol control solution, honokiol control solution, magnolol negative sample solution, control medicinal material solution and agilawood depression relieving tablet sample solution, and applying the strip sample points on the same high-efficiency silica gel G thin-layer plate with a volume ratio of 10:4, developing, taking out and airing the cyclohexane-acetone as developing agent, spraying a sulfuric acid ethanol solution of vanillin, heating the mixture until spots are clear in color development, and inspecting the mixture in sunlight;

the thin layer identification analysis of turmeric in the agilawood Shu Yupian comprises the following steps:

Grinding lignum Aquilariae Resinatum tablet into fine powder, adding anhydrous ethanol, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain sample solution; taking a proper amount of curcumin reference substance, adding methanol to prepare curcumin reference substance solution; ultrasonically treating Curcuma rhizome reference medicinal material with absolute ethanol, filtering, evaporating filtrate, and dissolving residue with methanol to obtain reference medicinal material solution; grinding a proper amount of turmeric negative sample into fine powder, adding absolute ethyl alcohol, and preparing turmeric negative sample solution by a test sample solution preparation method;

respectively sucking curcumin reference substance solution, mixing 1 μl of agilawood depression relieving tablet test substance solution and turmeric negative sample solution with the reference substance solution, and spotting in strip shape on the same high-efficiency silica gel G thin layer plate, wherein the volume ratio is 16:0.8:0.1, developing with chloroform-methanol-formic acid as developing agent, taking out, air drying, and inspecting in sunlight;

the thin-layer identification analysis of glycyrrhizin in agilawood Shu Yupian comprises the following steps:

grinding lignum Aquilariae Resinatum Yu Pian into fine powder, adding water, ultrasonic treating, centrifuging to obtain supernatant, filtering, extracting filtrate with ethyl acetate under shaking for 2 times, mixing ethyl acetate solutions, recovering solvent under reduced pressure to dry, and dissolving residue with methanol to obtain sample solution; adding methanol into appropriate amount of glycyrrhizin reference substance to obtain glycyrrhizin reference substance solution;

Respectively sucking a reference substance solution and a agilawood depression relieving tablet sample solution, and spotting the sample solutions in a strip shape on the same high-efficiency silica gel G thin layer plate, wherein the volume ratio is 15:1:1:2, developing ethyl acetate-formic acid-glacial acetic acid-water as developing agent, taking out, airing, spraying sulfuric acid ethanol solution for developing color when viewing, heating until the color of spots is clear, and then viewing under an ultraviolet lamp of 366 nm.

2. The method according to claim 1, wherein the thin layer chromatography of agalloch eaglewood Shu Yupian is performed by air drying the developed thin layer plate, spraying an alcohol sulfate solution containing vanillin, which consists of vanillin and 10wt% alcohol sulfate, and inspecting under sunlight, wherein the mass percentage of vanillin in the alcohol sulfate solution containing vanillin is 1wt%.

3. The method for detecting the thin layer chromatography of agalloch eaglewood Shu Yupian according to claim 1, wherein when the liquiritin is subjected to the thin layer identification analysis, the concentration of the sulfuric acid ethanol solution is 10wt%.

4. The thin layer chromatography detection method of agilawood Shu Yupian according to claim 1, further comprising the steps of a negative test and a durability test investigation.