Thin-layer chromatographic detection method for radix codonopsis and radix astragali stomach-invigorating granules

A technique of thin-layer chromatography and detection method is applied in the field of thin-layer chromatography detection of Shenqi Jianwei granules, which can solve the problem of inability to determine the active ingredients of Shenqi Jianwei granules, etc., and achieve the effect of accurate detection results.

Inactive Publication Date: 2019-02-01

ZHONGXING PHARM CO LTD JIANGSU

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Problems solved by technology

[0004] Purpose of the invention: In view of the above problems, the purpose of the present invention is to provide a TLC detection method...

Method used

4) compare the spots on the corresponding positions of the test product chromatogram and the reference substance chromatogram, and show the spots of the same color, which means that the Astragalus composition is contained in the Shenqi J...

Abstract

The invention discloses a thin-layer chromatographic detection method for radix codonopsis and radix astragali stomach-invigorating granules. The thin-layer chromatographic detection method for radixastragali comprises the following steps of 1) preparing a test solution, taking the radix codonopsis and radix astragali stomach-invigorating granules, performing washing with water-saturated n-butylalcohol, evaporating a combined n-butyl alcohol solution to dryness, adding methanol for dissolving obtained residues, performing arrangement on a neutral alumina column, performing eluting with the methanol, collecting eluant, performing evaporating to dryness, and adding the methanol for dissolving powder, so as to obtain the test solution; 2) preparing a reference solution; 3) applying samplesof the test solution and the reference solution to the same silica gel plate, and performing visual inspection under an ultraviolet lamp; and 4) comparing spots in the corresponding positions of a test color spectrum and a reference color spectrum, thereby indicating that the radix codonopsis and radix astragali stomach-invigorating granules contain the radix astragali component. The method has the advantages that the thin-layer chromatographic method is adopted for carrying out thin-layer chromatographic analysis on the radix astragali component in the radix codonopsis and radix astragali stomach-invigorating granules to detect whether the radix codonopsis and radix astragali stomach-invigorating granules contain the radix astragali component or not, so that the radix astragali componentis effectively detected and a detection result is accurate.

Application Domain

Component separation

Technology Topic

ChemistryThin layer chromatographic +6

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Examples

Experimental program(10)

Example Embodiment

[0046] Example 1

[0047] A thin-layer chromatography detection method for Shenqi Jianwei granules, including the thin-layer chromatography detection method for Astragalus membranaceus, specifically includes the following steps:

[0048] 1) Preparation of test solution: Take Shenqi Jianwei granules, grind them, add 50mL of water and reflux for 1h, filter, and evaporate the filter residue, add 50mL methanol, reflux for 1h, filter, and evaporate the filtrate to dryness, and add 30mL of water to dissolve the obtained powder , Shake and extract twice with water-saturated n-butanol. The amount of n-butanol saturated with water is 20mL each time. Combine the n-butanol solution and wash twice with the ammonia test solution. The amount of each ammonia test solution is 20mL. Wash twice with water-saturated n-butanol, each time the amount of water-saturated n-butanol is 20mL, remove the water liquid, evaporate the combined n-butanol liquid to dryness, add 5mL methanol to the obtained residue to dissolve, and place on neutral alumina On a column (100-200 mesh, 5g, 10-15mm), elute with 80 mL of methanol with a volume fraction of 40%, collect the eluate, evaporate to dryness, and dissolve the powder with 1 mL of methanol to obtain the test solution;

[0049] 2) Preparation of reference substance solution: take astragaloside IV reference substance and use methanol to make a solution containing 0.5mg/mL astragaloside IV reference substance to obtain a reference substance solution;

[0050] 3) Preparation of negative control solution: take a negative sample lacking astragalus, and use step 1) to obtain a negative control solution;

[0051] 4) Spot 10 μL of the test solution, 5 μL of the reference solution, and 10 μL of the negative control solution on the same silica gel G thin-layer plate with sodium carboxymethyl cellulose as a binder, using chloroform-methanol-water as Expand the developing agent, take it out, and dry it. Use a 10% sulfuric acid ethanol solution as the developer, heat it at 105°C until the spots are clearly colored, and inspect under an ultraviolet lamp (365nm). Among them, chloroform, The volume ratio of methanol to water is 13:7:2;

[0052] 5) Compare the spots on the corresponding positions of the chromatogram of the test substance and the reference substance, and show spots of the same color, that is, Shenqi Jianwei Granules contain astragalus components.

[0053] Test results such as figure 1 Shown, where figure 1 Among them, from left to right are negative samples, astragaloside IV reference substance, and batch numbers of 161001, 161002, and 161003. by figure 1 It can be seen that the negative samples have no interference, and this detection method can detect the astragalus components in Shenqi Jianwei Granules, and the detection method is accurate.

Example Embodiment

[0054] Example 2

[0055] A thin-layer chromatography detection method for Shenqi Jianwei granules, including the thin-layer chromatography detection method for Inulin, specifically includes the following steps:

[0056] 1) Preparation of test solution: Take 15g of Shenqi Jianwei Granules, grind it, add 25mL of dichloromethane, cold soak for 24h, filter, evaporate the filtrate, and add 1mL of dichloromethane to dissolve the residue to obtain the test solution;

[0057] 2) Preparation of reference substance mixed solution: take the reference substance of inulin and isoinulin, add the two in methanol to make the reference substance containing 2mg/mL inulin and 2mg/mL isoinulin To obtain the mixed solution of reference substance;

[0058] 3) Negative control solution preparation: take the negative sample lacking inulin, and use step 1) to obtain the negative control solution;

[0059] 4) Spot 10μL of the test solution, 10μL of the negative control solution, and 5μL of the reference mixed solution on the same silica gel G thin-layer plate with sodium carboxymethylcellulose as a binder, and apply petroleum ether at 60~90℃. Benzene-ethyl acetate is used as a developing agent. Expand twice, take it out, and dry. Use a 10% sulfuric acid ethanol solution as a developing agent. Heat at 108°C until the spots are clearly colored. Among them, 60~90°C petroleum The volume ratio of ether, benzene and ethyl acetate is 15:2:1;

[0060] 5) Compare the spots on the corresponding positions of the chromatogram of the test substance and the reference substance, and show spots of the same color, that is, the Shenqi Jianwei Granules contain elegans.

[0061] Test results such as figure 2 Shown, where figure 2 In the middle, from left to right are the samples with batch numbers 161001 and 161002, the mixed solution of reference substance, the samples with batch number 161003, and the negative samples. by figure 2 It can be seen that the negative samples have no interference, and this detection method can detect the elegans in Shenqi Jianwei granules, and the detection method is accurate.

Example Embodiment

[0062] Example 3

[0063] A thin-layer chromatography detection method for Shenqi Jianwei granules, including the thin-layer chromatography detection method for Angelica sinensis, specifically includes the following steps:

[0064] 1) Preparation of test solution: Take 15g of Shenqi Jianwei Granules, add diethyl ether and extract twice, each time 20mL of diethyl ether, combine diethyl ether solution, evaporate to dryness at low temperature, add 1mL of ethyl acetate to dissolve the residue to obtain the test product Solution

[0065] 2) Preparation of control medicinal material solution: Take 0.25g of Angelica sinensis control medicinal material and add 2 mL of ether, shake for 10 min, and let stand still, and take the supernatant as the control medicinal material solution;

[0066] 3) Preparation of negative control solution: Take the negative sample of Angelica sinensis and prepare the negative control solution by the method in step 1);

[0067] 4) Spot 5μL each of the test solution, control medicinal solution, and negative control solution on the same silica gel plate, use n-hexane-ethyl acetate as the developing agent, unfold, take out, dry, and inspect under UV light. Among them, the volume ratio of n-hexane and ethyl acetate is 9:1;

[0068] 5) Compare the spots on the corresponding positions of the chromatogram of the test product and the chromatogram of the control medicinal materials, and show the spots of the same color, that is, the Shenqi Jianwei Granule contains the components of Angelica.

[0069] Test results such as image 3 Shown, where image 3 In the middle, from left to right are negative samples, batch numbers 161001, 161002, 161003 three samples, and Angelica reference medicine. by image 3 It can be seen that the negative sample has no interference, and this detection method can detect the Angelica component in Shenqi Jianwei Granules, and the detection method is accurate.

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Thin-layer chromatographic detection method for radix codonopsis and radix astragali stomach-invigorating granules

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