A method for constructing a characteristic spectrum of detoxification capsules

Abstract

The present invention relates to the field of medical technology, and more particularly to a method for constructing a characteristic spectrum for detoxification capsules. The present invention improves existing detoxification capsule quality standards by enabling simultaneous detection of chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde. Furthermore, the components of the formulation, such as chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde, are controlled, further ensuring the safety, uniformity, stability, and controllability of the product quality.

Description

Technical Field

[0001] The present invention relates to the field of medical technology, and in particular to a method for constructing a characteristic spectrum of a detoxification capsule. Background Art

[0002] Heat-clearing and detoxification is a type of treatment in Traditional Chinese Medicine (TCM). It is a treatment method that uses a prescription composed mainly of drugs with cooling and detoxifying effects to treat various heat-toxic diseases. It is suitable for treating plague, febrile diseases, and various heat-toxic diseases or sores, carbuncles, and furuncles. Symptoms include high fever, restlessness, dry mouth and throat, constipation and yellow urine, or vomiting and bleeding, or redness, swelling, heat and pain, red tongue with yellow coating, and a rapid and strong pulse. Infectious diseases are often caused by exogenous toxins, leading to a series of symptoms such as fever, sores, pus, etc. Therefore, heat-clearing and detoxification is often used to treat infectious diseases. Infectious diseases can occur in people of all ages. Bacteria, viruses, mycoplasmas, fungi, and parasites are often the causes of infectious diseases, and the vast majority of infectious diseases are caused by viral infections.

[0003] The specific prescription of the compound Chinese medicine of the detoxification capsule is composed of 35 medicinal materials, including animal treasure, turnip paste, earthworm mustard, strychnine (processed), water cypress branch, borax (processed), pearl (processed), coral, lapis lazuli (processed), turquoise (processed), iron powder (processed), ring copper (processed), stone flower (processed), rock essence paste, nutmeg, amomum villosum, rhizoma dahliae, safflower, clove, terminalia chebula, pokeweed, sandalwood, rosewood, artificial musk, artificial bezoar, thorny bezoar, calamus, cardamom, pterygium wilfordii, Sichuan small yellow chamomile, drynaria, sweet pine, flat-leaved coral disc, white gentian, and moss pedicularis. These medicinal materials are taken from high altitude areas, with little pollution and strong efficacy. They have good effects of clearing away heat and detoxifying, removing dead tissue and promoting tissue regeneration.

[0004] The existing quality standards for the Jiedu Capsule compound Chinese medicine do not include a characteristic spectrum study. This is because the compound Chinese medicine contains numerous medicinal ingredients, making extraction and separation difficult. The present invention can simultaneously effectively control the components of chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde in the Jiedu Capsule compound Chinese medicine, thereby improving the quality control level of the Jiedu Capsule. Summary of the Invention

[0005] In order to make up for the deficiencies of the prior art, the present invention provides a method for constructing a characteristic spectrum of a detoxification capsule.

[0006] The present invention is achieved through the following technical solutions:

[0007] The present invention provides a method for constructing a characteristic spectrum of a detoxification capsule, which can simultaneously detect terminal acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde; the method comprises the following steps:

[0008] Step 1: Preparation of test solution

[0009] 5 g of the compound Chinese medicine of Jiedu Capsule was taken, 50 mL of petroleum ether with a boiling range of 60-90 ° C was added, and ultrasonic treatment was carried out at 500W / 40kHz for 30 minutes. The filtrate was discarded to obtain a residue; an equal volume of a mixed upper and lower phase solution after layering of n-hexane-ethyl acetate-methanol-water in a volume ratio of 4:5:4:5 was added to the residue to dissolve the residue, and then the residue was injected into a high-speed countercurrent chromatography at a speed of 1000 r / min, a flow rate of 2.5 mL / min, and a detection wavelength of 240 nm. The effluent from 100 min to 200 min was collected and dried under reduced pressure at low temperature; then, an acetonitrile-water solution with a volume ratio of 1:1 was added to the product obtained by vacuum drying to dissolve it, and the product was purified by chromatography on a C18 column (10.0 mm × 250 mm, 5μm) was prepared using an acetonitrile-0.2% phosphoric acid solution as the mobile phase, with a gradient elution ratio of 40:60→70:30, 0-40 min, a flow rate of 2.0 mL / min, and a detection wavelength of 240 nm. The effluent was collected after 15 min to 25 min, and the effluents were combined and dried under reduced pressure at low temperature to obtain a dry product. 5 mL of methanol was added to the dry product for dissolution, and the product was purified by passing it through a C18 solid phase extraction column, sequentially eluting with 5 mL of 20% methanol aqueous solution and 5 mL of 80% methanol aqueous solution. The eluted product was blown to dryness with liquid nitrogen. The residue was redissolved in a methanol solution containing 0.1% formic acid and filtered through a 0.22 μm organic filter membrane to obtain the product.

[0010] Step 2: Preparation of reference solution

[0011] Take appropriate amount of terminalic acid reference substance, syringin reference substance, kaempferol-30-rutinoside reference substance, β-asarone reference substance, and asaraldehyde reference substance, accurately weigh them, add methanol to make a solution containing 120 μg per 1 ml, shake well, and use it as the reference substance solution;

[0012] Step 3: Detection according to the following HPLC conditions

[0013] Octadecylsilane bonded silica gel was used as the filler; acetonitrile-methanol-tetrahydrofuran (6:3:1, by volume) was used as the mobile phase A, and 10 mM potassium dihydrogen phosphate-5 mM ammonium acetate buffer (pH 4.0) was used as the mobile phase B for gradient elution; the flow rate was 1 ml per minute; the column temperature was 30°C; detection was performed with a diode array detector at a wavelength of 240 nm; the number of theoretical plates calculated based on the chebulic acid peak was not less than 5000.

[0014] The gradient elution program is as follows:

[0015] From 0 to 15 min, the volume ratio of phase A:phase B changed from 2:98 to 12.5:87.5;

[0016] From 15 to 40 min, the volume ratio of phase A:phase B changed from 12.5:87.5 to 35:65;

[0017] From 40 to 70 min, the volume ratio of phase A:phase B changed from 35:65 to 59:41;

[0018] From 70 to 93 min, the volume ratio of phase A:phase B changed from 59:41 to 80:20;

[0019] From 93 to 95 min, the volume ratio of phase A:phase B changed from 80:20 to 2:98;

[0020] 95-105 min, the volume ratio of phase A:phase B is 2:98;

[0021] Step 4: Generate a control feature map.

[0022] Preferably, in step three, the column length is 250 mm, the inner diameter is 4.6 mm, and the particle size is 5 μm.

[0023] Preferably, the peak corresponding to the peak of the chebulic acid reference substance is taken as the S peak, and the relative retention time of each characteristic peak and the S peak is calculated, and the relative retention time is within the range of ±10% of the specified value; the test sample chromatogram presents 11 characteristic peaks, of which peak 1 is chebulic acid; peak 4 is syringin, with a relative retention time of 2.31; peak 6 is kaempferol-30-rutinoside, with a relative retention time of 7.31; peak 8 is β-asarone, with a relative retention time of 8.43; peak 9 is asaraldehyde, with a relative retention time of 8.89.

[0024] Compared with the prior art, the present invention has the following advantages:

[0025] The present invention improves the quality standard of the compound traditional Chinese medicine of Jiedu Capsule, realizes the simultaneous detection of chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde. In addition, the components such as chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde in the preparation are controlled, further ensuring the safety, uniformity, stability, and controllable quality of the product, thereby ensuring its clinical efficacy and the health of a large number of patients. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The present invention will be further described below with reference to the accompanying drawings.

[0027] Figure 1 The chromatograms of eight batches of compound Chinese medicine samples containing Terminalia chebula and Clove are as follows: S1: 01240714; S2: 01240715; S3: 01240716; S4: 01240411; S5: 01240412; S6: 01240413; S7: 01240515; S8: 01240516;

[0028] Figure 2 This is a comparative characteristic spectrum of compound Chinese medicine containing Terminalia chebula and clove. DETAILED DESCRIPTION

[0029] The present invention will be further described below with reference to the accompanying drawings.

[0030] Example 1

[0031] The method for constructing the characteristic spectrum of Jiedu Capsule is as follows:

[0032] (1) Take 5g of the compound Chinese medicine content of Jiedu Capsule, add 50mL of petroleum ether with a boiling range of 60~90℃, and ultrasonically treat for 30 minutes at 500W / 40kHz. Discard the filtrate; add equal volumes of the upper and lower phase solution after the mixture of n-hexane-ethyl acetate-methanol-water with a volume ratio of 4:5:4:5 to dissolve the residue, inject it into the high-speed countercurrent chromatography, rotate at 1000 r / min, flow rate at 2.5mL / min, detection wavelength at 240nm, collect the effluent from 100min to 200min, dry under reduced pressure at low temperature, and obtain the crude extract of Chinese medicine. The specific steps are as follows:

[0033] Liquid preparation: Ultrasonic degassing for about 20 minutes, after degassing, let it stand and cool to room temperature before pumping the liquid.

[0034] Turn on the thermostatic water bath and raise the temperature to the set temperature.

[0035] Pump the stationary phase: Pump in the stationary phase at a flow rate of 2.5 ml / min. Stop the pump when about 20 to 50 ml of the stationary phase flows out of the detector outlet.

[0036] Balance: Turn on the UV detector and start preheating, rotate the main unit forward to 1000rpm (FWD is forward, REV is reverse), and pump in the mobile phase at a flow rate of 2.5ml / min. When the mobile phase flows out of the outlet and the UV signal is stable, the system is basically balanced.

[0037] Injection: Dissolve a certain amount of sample in the upper and lower phases of the system. After ultrasonic dissolution, pour the sample solution into the sample syringe, switch the six-way injection valve to load, push out the bubbles and aspirate the liquid until the sample enters the injection circle. Switch load to inject, adjust the detector and workstation to zero and start recording.

[0038] Receive flow: record at the workstation, collect data after saving, and save.

[0039] Cleaning: Disconnect the pump from the main unit, connect the main unit inlet to the air pipe outlet, and blow air; after blowing out the solvent in the main unit, pump in about 50ml of cleaning liquid, blow air, and repeat this process 2 to 3 times; the last time, blow air for a long time (about 1 hour until it is dry) to blow out all the liquid in the main unit.

[0040] Turn off the computer.

[0041] The crude extract was dissolved in an acetonitrile-water solution with a volume ratio of 1:1 and prepared on a C18 column (10.0 mm × 250 mm, 5 μm). The mobile phase was acetonitrile-0.2% phosphoric acid solution with gradient elution (40:60→70:30, 0-40 min) at a flow rate of 2.0 mL / min and a detection wavelength of 240 nm. The effluent from 15 min to 25 min was collected, combined, and dried under reduced pressure at low temperature. The dried product was dissolved in 5 mL of methanol and purified on a C18 solid-phase extraction column, sequentially eluted with 5 mL of 20% methanol-water solution and 5 mL of 80% methanol-water solution. The eluted product was blown to dryness with liquid nitrogen. The residue was re-dissolved in a methanol solution containing 0.1% formic acid and passed through a 0.22 μm organic filter membrane to obtain the test sample.

[0042] Example 2

[0043] 1. Equipment and Materials

[0044] .

[0045] 2. Reagents and test drugs

[0046] .

[0047] 3. Sample information

[0048] .

[0049] 4. Test and inspection

[0050] 4.1 Chromatographic conditions and system suitability test

[0051] Octadecylsilane bonded silica gel was used as the packing (column length, 250 mm, inner diameter, 4.6 mm, particle size, 5 μm); mobile phase A was acetonitrile-methanol-tetrahydrofuran (volume ratio, 6:3:1); mobile phase B was 10 mM potassium dihydrogen phosphate-5 mM ammonium acetate buffer (pH 4.0), using gradient elution as specified in the table below; the flow rate was 1 ml / min; the column temperature was 30°C; and the detection wavelength was 240 nm. The number of theoretical plates, calculated based on the chebulic acid peak, should be no less than 5000.

[0052] .

[0053] Preparation of reference solution

[0054] Take appropriate amount of terminalic acid reference substance, syringin reference substance, kaempferol-30-rutinoside reference substance, β-asarone reference substance, and asaraldehyde reference substance, accurately weigh them, add methanol to make a solution containing 120 μg per 1 ml, shake well, and use it as the reference substance solution.

[0055] Preparation of test solution

[0056] 5 g of the detoxification capsule contents were added to 50 mL of petroleum ether with a boiling range of 60-90°C, and ultrasonicated at 500W / 40kHz for 30 min. The filtrate was discarded. The residue was dissolved in an equal volume of a mixture of n-hexane-ethyl acetate-methanol-water (4:5:4:5 by volume) and injected into a high-speed countercurrent chromatograph at a speed of 1000 r / min, a flow rate of 2.5 mL / min, and a detection wavelength of 240 nm. The effluent from 100 min to 200 min was collected and dried under reduced pressure at low temperature. The residue was dissolved in an acetonitrile-water solution with a volume ratio of 1:1 and prepared on a C18 column (10.0 mm × 250 mm, 5 μm) with a mobile phase of acetonitrile-0.2% phosphoric acid solution in a gradient elution (40:60→70:30, 0-40 min) at a flow rate of 2.0 mL / min and a detection wavelength of 240 nm. The effluent from 15 min to 25 min was collected and combined and dried under reduced pressure at low temperature. The dried product was added to a 5% HPLC column. The product was dissolved in 100 mL of methanol and purified by C18 solid phase extraction column, followed by elution with 5 mL of 20% methanol aqueous solution and 5 mL of 80% methanol aqueous solution. The eluted product was blown to dryness with liquid nitrogen. The residue was redissolved in methanol solution containing 0.1% formic acid and filtered through a 0.22 μm organic filter membrane to obtain the test solution.

[0057] Assay

[0058] Accurately pipette 10 μl of reference solution and test solution respectively, inject into liquid chromatograph, measure, and record the chromatogram.

[0059] 4.2 Precision

[0060] Take 1 g of the compound Chinese medicine containing Terminalia chebula and Clove (Batch No.: 01240714), prepare the test solution according to the test solution preparation method under "4.1", inject 6 times according to the chromatographic conditions under "4.1", record the chromatogram, measure the relative retention time and relative peak area of ​​each chromatographic peak, and calculate the RSD.

[0061] Table 1 Precision relative retention time results

[0062] .

[0063] Table 2 Precision relative peak area results

[0064] .

[0065] The results showed that the relative retention time RSDs of each chromatographic peak were less than 1.0%, and the relative peak area RSDs were less than 10.0%, indicating good precision.

[0066] 4.3 Repeatability

[0067] Take 1 g of the compound Chinese medicine containing Terminalia chebula and Clove (Batch No.: 01240714), and make 6 portions. Prepare the test solution according to the test solution preparation method under "4.1". Inject the sample according to the chromatographic conditions under "4.1", record the chromatogram, measure the relative retention time and relative peak area of ​​each chromatographic peak, and calculate the RSD.

[0068] Table 3 Repeatability relative retention time results

[0069] .

[0070] Table 4 Repeatability relative peak area results

[0071] .

[0072] The results showed that the relative retention time RSDs of each chromatographic peak were less than 1.0%, and the relative peak area RSDs were less than 10.0%, indicating good repeatability.

[0073] 4.4 Stability

[0074] Take 1 g of the compound Chinese medicine containing Terminalia chebula and Clove (Batch No.: 01240714), prepare the test solution according to the test solution preparation method under "4.1", and inject the sample at 0 h, 2 h, 4 h, 8 h, 12 h, and 24 h according to the chromatographic conditions under "3.1", record the chromatogram, measure the relative retention time and relative peak area of ​​each chromatographic peak, and calculate the RSD.

[0075] Table 5 Stability relative retention time results

[0076] .

[0077] Table 6 Stability relative peak area results

[0078] .

[0079] The results showed that the relative retention time RSDs of each chromatographic peak were less than 1.0%, and the relative peak area RSDs were less than 10.0%, indicating that the solution had good stability.

[0080] In summary, the method demonstrated good precision in the precision test, with the relative retention time RSDs for each chromatographic peak less than 1.0% and the relative peak area RSDs less than 10.0%. In the repeatability test, the relative retention time RSDs for each chromatographic peak were less than 1.0% and the relative peak area RSDs less than 10.0%, indicating good repeatability. In the stability test, the relative retention time RSDs for each chromatographic peak were less than 1.0% and the relative peak area RSDs less than 10.0%, indicating good solution stability. This method has been methodologically validated and the results are reliable and accurate.

[0081] Example 3 Construction of the control characteristic spectrum of Jiedu Capsules

[0082] Chromatographic conditions and system suitability test

[0083] Octadecylsilane bonded silica gel was used as the packing (column length, 250 mm, inner diameter, 4.6 mm, particle size, 5 μm); mobile phase A was acetonitrile-methanol-tetrahydrofuran (volume ratio, 6:3:1); mobile phase B was 10 mM potassium dihydrogen phosphate-5 mM ammonium acetate buffer (pH 4.0), using gradient elution as specified in the table below; the flow rate was 1 ml / min; the column temperature was 30°C; and the detection wavelength was 240 nm. The number of theoretical plates, calculated based on the chebulic acid peak, should be no less than 5000.

[0084] .

[0085] Preparation of reference solution

[0086] Take appropriate amount of terminalic acid reference substance, syringin reference substance, kaempferol-30-rutinoside reference substance, β-asarone reference substance, and asaraldehyde reference substance, accurately weigh them, add methanol to make a solution containing 120 μg per 1 ml, shake well, and use it as the reference substance solution.

[0087] Preparation of test solution: 5 g of the compound Chinese medicine content of Jiedu Capsule was added to 50 mL of petroleum ether with a boiling range of 60-90 ° C, and ultrasonicated at 500W / 40kHz for 30 minutes, and the filtrate was discarded; the residue was dissolved in an equal volume of a mixture of n-hexane-ethyl acetate-methanol-water with a volume ratio of 4:5:4:5, and the upper and lower phases were mixed after layering, and injected into a high-speed countercurrent chromatograph at a speed of 1000 r / min, a flow rate of 2.5 mL / min, and a detection wavelength of 240 nm. The effluent from 100 min to 200 min was collected and dried under reduced pressure at low temperature; the effluent was dissolved in an acetonitrile-water solution with a volume ratio of 1:1, and the effluent was purified by chromatography on a C18 column (10.0 mm × 250 mm, 5μm) with an acetonitrile-0.2% phosphoric acid solution as the mobile phase, gradient elution (40:60→70:30, 0-40min), a flow rate of 2.0 mL / min, and a detection wavelength of 240 nm. The effluent from 15min-25min was collected, combined, and dried under reduced pressure at low temperature. The dried product was dissolved in 5 mL of methanol and purified by a C18 solid-phase extraction column, sequentially washed with 5 mL of 20% methanol aqueous solution and 5 mL of 80% methanol aqueous solution. The eluted product was blown to dryness with liquid nitrogen. The residue was redissolved in a methanol solution containing 0.1% formic acid and filtered through a 0.22 μm organic filter membrane to obtain the product.

[0088] Assay

[0089] Accurately pipette 10 μl of reference solution and test solution respectively, inject into liquid chromatograph, measure, and record the chromatogram.

[0090] According to item "4.1", the chromatograms of 8 batches of compound Chinese medicine containing terminalia chebula and clove were imported into the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System". The chromatographic peaks that existed in the chromatograms of compound Chinese medicine containing terminalia chebula and clove from different batches were selected as common peaks; the reference characteristic spectrum was generated using the average calculation method, and the relative retention time and relative peak area of ​​each common peak were calculated. See the attached Figure 1 、 2 .

[0091] Table 7 Relative retention time results of eight batches of compound Chinese medicine samples containing Terminalia chebula and Clove

[0092] .

[0093] Table 8 Relative peak area results of eight batches of compound Chinese medicine samples containing Terminalia chebula and cloves

[0094] .

[0095] The chromatograms of 8 batches of compound Chinese medicine samples containing Terminalia chebula and Clove showed 11 common peaks. The RSDs of the relative retention times of the 11 common peaks were all less than 1.0%, and the RSDs of the relative peak areas were all less than 10.0%.

[0096] The test sample chromatogram shows 11 characteristic peaks, of which Peaks 1, 4, 6, 8, and 9 should correspond to the peaks of the chebulic acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde reference substance, respectively. The peak corresponding to the chebulic acid reference substance peak is the S peak. Calculate the relative retention time of each characteristic peak to the S peak, and the relative retention time should be within ±10% of the specified value. The specified values ​​are: 1.74 (peak 2), 2.18 (peak 3), 2.31 (peak 4), 5.05 (peak 5), 7.31 (peak 6), 7.76 (peak 7), 8.43 (peak 8), 8.89 (peak 9), 9.51 (peak 10), and 10.15 (peak 11).

Claims

1. A method for constructing a characteristic spectrum of a detoxification capsule, characterized in that: The method can simultaneously detect terminalia acid, syringin, kaempferol-30-rutinoside, β-asarone, and asaraldehyde; and comprises the following steps: Step 1: Preparation of test solution 5 g of the compound Chinese medicine content of Jiedu Capsule was taken, petroleum ether was added, and after ultrasonic treatment, the filtrate was discarded to obtain a residue; the obtained residue was added with equal volumes of the upper and lower phase solutions after mixing and layering n-hexane-ethyl acetate-methanol-water to dissolve the residue, and injected into a high-speed countercurrent chromatograph at a speed of 1000 r / min, a flow rate of 2.5 mL / min, and a detection wavelength of 240 nm. The effluent from 100 min to 200 min was collected, and the crude extract was dried under reduced pressure at low temperature to obtain a crude extract; an acetonitrile-water solution with a volume ratio of 1:1 was added to the crude extract to dissolve the crude extract, and the crude extract was prepared on a C18 column with an acetonitrile-0.2% phosphoric acid solution as the mobile phase, a gradient elution program of 40:60→70:30, 0-40 min, a flow rate of 2.0 mL / min, and a detection wavelength of 240 nm. The effluent from 15 min to 25 min was collected, and the effluents were combined and dried under reduced pressure at low temperature to obtain a dry product; 5 mL of methanol was added to the dry product to dissolve the product, and the product was purified by a C18 solid phase extraction column, and then 5 mL The sample was washed with 20% methanol solution and eluted with 5 mL of 80% methanol solution. The eluted solution was blown to dryness with liquid nitrogen. The residue was redissolved with methanol solution containing 0.1% formic acid and filtered through a 0.22 μm organic filter membrane to obtain the test solution. Step 2: Preparation of reference solution Take appropriate amount of terminalic acid reference substance, syringin reference substance, kaempferol-30-rutinoside reference substance, β-asarone reference substance, and asaraldehyde reference substance, accurately weigh them, add methanol to make a solution containing 120 μg per 1 ml, shake well, and use it as the reference substance solution; Step 3: Detection according to the following HPLC conditions Octadecylsilane bonded silica gel was used as the filler; acetonitrile-methanol-tetrahydrofuran (6:3:1, by volume) was used as the mobile phase A, and 10 mM potassium dihydrogen phosphate-5 mM ammonium acetate buffer (pH 4.0) was used as the mobile phase B for gradient elution; the flow rate was 1 ml per minute; the column temperature was 30°C; detection was performed with a diode array detector at a wavelength of 240 nm; the number of theoretical plates calculated based on the chebulic acid peak was not less than 5000. The gradient elution program is as follows: From 0 to 15 min, the volume ratio of phase A:phase B changed from 2:98 to 12.5:87.5; From 15 to 40 min, the volume ratio of phase A:phase B changed from 12.5:87.5 to 35:65; From 40 to 70 min, the volume ratio of phase A:phase B changed from 35:65 to 59:41; From 70 to 93 min, the volume ratio of phase A:phase B changed from 59:41 to 80:20; From 93 to 95 min, the volume ratio of phase A:phase B changed from 80:20 to 2:98; 95-105 min, the volume ratio of phase A:phase B is 2:98; Step 4: Generate a control feature map.

2. The method for constructing a characteristic spectrum of a detoxification capsule according to claim 1, characterized in that: In step 1, after adding petroleum ether, ultrasonic treatment was performed at 500W / 40kHz for 30 minutes.

3. The method for constructing a characteristic spectrum of a detoxification capsule according to claim 1, characterized in that: In step 1, the amount of petroleum ether added is 50 mL, and the boiling range is 60~90℃.

4. The method for constructing a characteristic spectrum of a detoxification capsule according to claim 1, characterized in that: In step 1, the volume ratio of the upper and lower phase solutions of equal volume mixed after the added n-hexane-ethyl acetate-methanol-water mixture is 4:5:4:

5.

5. The method for constructing a characteristic spectrum of a detoxification capsule according to claim 1, characterized in that: In step 1, the C18 chromatographic column was 10.0 mm × 250 mm, 5 μm.

6. The method for constructing a characteristic spectrum of a detoxification capsule according to claim 1, characterized in that: In step 3, the column length is 250 mm, the inner diameter is 4.6 mm, and the particle size is 5 μm.

7. A method for constructing a characteristic spectrum of a detoxification capsule according to any one of claims 1 to 6, characterized in that: The peak corresponding to the peak of the chebulic acid reference substance was taken as the S peak, and the relative retention time of each characteristic peak and the S peak was calculated. The relative retention times were all within the range of ±10% of the specified value; the chromatogram of the test sample showed a total of 11 characteristic peaks, among which Peak 1 was chebulic acid; Peak 4 was syringin, with a relative retention time of 2.31; Peak 6 was kaempferol-30-rutinoside, with a relative retention time of 7.31; Peak 8 was β-asarone, with a relative retention time of 8.43; Peak 9 was asaraldehyde, with a relative retention time of 8.89.

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