Quality detection method of dehumidification guling decoction
By using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-Q-TOF-MS) and macroporous adsorption resin column treatment, the problem of insufficient quality monitoring of Chushi Weiling Decoction was solved, enabling comprehensive analysis and quality control of the components of Chushi Weiling Decoction, and ensuring the stability and reliability of the medicine.
Patent Information
- Application Number
- CN202411366543.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-12-12
- Estimated Expiration
- 2044-09-27
AI Technical Summary
Existing technologies cannot comprehensively monitor the quality of Chushi Weiling Decoction, nor can they perform qualitative analysis of its chemical components, resulting in an inability to fully control the quality of Chushi Weiling Decoction.
Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-Q-TOF-MS) was used to perform qualitative analysis of the dehumidifying stomach-soothing decoction through gradient elution and specific mass spectrometry conditions. The sample was then processed using a macroporous adsorption resin column to obtain first-order and multi-order mass spectrometry information for each compound.
This study enabled the simultaneous detection of almost all medicinal components in Chushi Weiling Decoction, providing a scientific basis, ensuring the quality stability and controllability of Chushi Weiling Decoction, preventing counterfeiting incidents, and supporting research on pharmacodynamic activity.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of drug detection, in particular to a quality detection method of Dushi Weiling decoction. BACKGROUND
[0002] Dushi Weiling decoction is from the fourth volume of "Orthodox Surgery", which has the effects of clearing heat and removing dampness, and invigorating spleen and promoting diuresis. It is mainly used for treating damp-heat obstruction of spleen and lung, causing fire and redness, and causing pain. It is also used for treating yellow-white color and different size of water blisters, and causing pain.
[0003] Dushi Weiling decoction is mainly made of Chenpi, Zhizi, Fangfeng, Jianghoupu, Futo Cangzhu, Zhuling, Zexie, Chizhudi, Tuocha Baishu, Mutong, Huashi, Gancao and Rougui, each one coin, water two cups, and 20 roots of lampwick (1.5m), which is boiled for eight minutes and taken before eating.
[0004] The ultra-high performance liquid chromatography tandem mass spectrometry technology has high analysis efficiency and speed, and can obtain accurate molecular structure information, and can obtain the first and multi-level mass spectrum information of each compound, which provides a good technical means for multi-index component analysis of complex traditional Chinese medicine system. Dushi Weiling decoction is made of 14 kinds of traditional Chinese medicines, and the components are extremely complex. At present, the quality of Dushi Weiling decoction cannot be comprehensively monitored, and the chemical components contained in Dushi Weiling decoction cannot be qualitatively analyzed. Therefore, it is necessary to develop a quality detection method of Dushi Weiling decoction, so as to more comprehensively detect the quality of Dushi Weiling decoction. SUMMARY
[0005] In view of the above problems, the present application provides a quality detection method of Dushi Weiling decoction.
[0006] To achieve the above purpose, the technical scheme adopted by the present application is:
[0007] A quality detection method of Dushi Weiling decoction, the quality detection method comprises the following steps:
[0008] S1, taking Dushi Weiling decoction to prepare a test solution;
[0009] S2, taking the test solution to detect the quality of Dushi Weiling decoction by ultra-high performance liquid chromatography tandem mass spectrometry;
[0010] The mobile phase A of the ultra-high performance liquid chromatography detection is acetonitrile, and the mobile phase B is a 0.08-0.12wt% formic acid aqueous solution;
[0011] The elution mode of the ultra-high performance liquid chromatography detection is gradient elution;
[0012] The elution conditions of the gradient elution are:
[0013] 0–15 min, 8% → 20% mobile phase A, 92% → 80% mobile phase B;
[0014] 15–22 min, 20% → 37% mobile phase A, 80% → 63% mobile phase B;
[0015] 22–27 min, 37% → 70% mobile phase A, 63% → 30% mobile phase B;
[0016] 27–29 min, 70% → 8% mobile phase A, 30% → 92% mobile phase B.
[0017] Furthermore, the test solution is prepared by passing the dehumidifying Weiling Decoction liquid through a macroporous adsorption resin column, washing with water, discarding the water, eluting with an ethanol aqueous solution, collecting the eluent, evaporating it to dryness in a water bath, dissolving the residue in a methanol aqueous solution, shaking well, filtering, and so on.
[0018] Furthermore, the concentration of the ethanol-water solution used for elution is 90–98 vol%, and the volume is 45–60 mL.
[0019] Furthermore, the concentration of the methanol-water solution used for dissolution is 40–60 vol%.
[0020] Furthermore, the liquid form of the dampness-removing Weiling Decoction is made by dissolving the dry powder of the dampness-removing Weiling Decoction in water;
[0021] Alternatively, it can be prepared by diluting the concentrated Weiling Decoction for Dampness Removal with water.
[0022] Alternatively, the decoction of Weiling Decoction for Removing Dampness can be used directly as the liquid form of Weiling Decoction for Removing Dampness;
[0023] When the dry powder of the dehumidifying stomach-soothing decoction is dissolved in water to prepare the liquid dehumidifying stomach-soothing decoction, the weight-to-volume ratio of the dry powder of the dehumidifying stomach-soothing decoction to the prepared test solution is 0.064-0.096 g: 1 mL;
[0024] When the concentrated dehumidifying Weiling Decoction is diluted with water to prepare the dehumidifying Weiling Decoction liquid, the volume ratio of the concentrated dehumidifying Weiling Decoction to the prepared test solution is 0.8-1.2 mL:1 mL.
[0025] When the decoction of Weiling Decoction is used directly as the liquid of Weiling Decoction, the volume ratio of the decoction of Weiling Decoction to the prepared test solution is 4-6 mL: 1 mL.
[0026] Furthermore, the mass spectrometry detection is performed in both positive ion mode and negative ion mode.
[0027] Furthermore, the mass spectrometry detection conditions are as follows: drying gas temperature 345–355°C, drying gas flow rate 8–12 L / min, nebulizing gas pressure 34–36 psi, sheath gas temperature 345–355°C, sheath gas flow rate 11–13 L / min, capillary voltage in positive ion mode 3900–4100 V, and capillary voltage in negative ion mode 3400–3600 V.
[0028] Furthermore, during the mass spectrometry detection process, the first-stage mass spectrometry uses MS mode with a mass scan range of 100–1200 m / z, and the second-stage mass spectrometry uses Auto MSMS.
[0029] Furthermore, the detection wavelength of the ultra-high performance liquid chromatography is 260–270 nm.
[0030] Furthermore, the ultra-high performance liquid chromatography column temperature is 40–50 °C and the flow rate is 0.3–0.5 mL / min.
[0031] The beneficial effects of the quality testing method for the dehumidifying and stomach-strengthening decoction of the present invention are as follows:
[0032] This invention uses UPLC-Q-TOF-MS to qualitatively analyze the chemical composition of the material basis of Chushi Weiling Decoction, providing a scientific basis for the study of the material basis of Chushi Weiling Decoction and clarifying its main chemical composition.
[0033] This invention employs UPLC-Q-TOF-MS to qualitatively analyze the chemical composition of the reference material for Chushi Weiling Decoction. The analysis is highly efficient and fast, and can obtain accurate molecular structure information of Chushi Weiling Decoction. It can also obtain first-order and multi-order mass spectrometry information of each compound, providing a good technical means for the multi-index component analysis of Chushi Weiling Decoction, a complex traditional Chinese medicine system.
[0034] This invention employs UPLC-Q-TOF-MS to qualitatively analyze the chemical composition of the reference substance for Chushi Weiling Decoction, providing a scientific basis for the study of the material basis of Chushi Weiling Decoction and clarifying its main chemical composition.
[0035] The quality testing method of this invention can detect almost all the medicinal ingredients in the whole formula of Chushi Weiling Decoction;
[0036] This invention achieves the goal of effectively separating different effective components of the dehumidifying stomach-soothing decoction by changing the elution system and utilizing the different physicochemical properties of the different effective components in the dehumidifying stomach-soothing decoction.
[0037] By selecting specific chromatographic and mass spectrometric conditions, this invention can obtain a better chromatogram of the dampness-removing Weiling Decoction.
[0038] The quality testing method of the present invention also has good feasibility, stability and reproducibility;
[0039] The quality detection method of this invention can detect and clarify the medicinal flavor source and qualitative analysis of 37 peak substances. Among them, 13 flavonoids were identified, namely glucosyl apigenin, glycyrrhizin, apigenin glycyrrhizin, rutin, rutin, hesperidin, styracin, isoglycyrrhizin, limonene, glucosyl apigenin, hesperidin, 3,5,6,7,3',4',5'-heptamethoxyflavone, and 5,6,7,8,4'-pentamethoxyflavone, which are attributed to tangerine peel and licorice, respectively. Two phenolic compounds were identified, namely honokiol and magnolol, both unique to Magnolia officinalis. Two alkaloids were identified, namely magnoflorine and magnolol, both attributed to Magnolia officinalis. Five iridoids were identified, namely geniposide B and jasminoside. B. Geniposide-1-gentiopicroside, geniposide, and ′-O-p-coumaryl quercetin gentiopicroside were all classified as belonging to Gardenia jasminoides. Four chromogenone compounds were identified: cimicifugin glycoside, cimicifugin, 5-O-methylvisamidol glycoside, and scutellarin glycoside, all classified as belonging to Saposhnikovia divaricata. Two saponin compounds were identified: glycyrrhizin G2 and glycyrrhizic acid, both classified as belonging to Glycyrrhiza uralensis. Two lignan compounds were identified: magnolinoside B and magnolinoside G2. Glycoside A was identified, all belonging to Magnolia officinalis; three terpenoids were identified: Akebia quinata glycoside B, Crocinosin I, and 16-oxoallotin A, belonging to Akebia quinata, Gardenia jasminoides, and Alisma plantago-aquatica, respectively; one organic acid ester was identified, 4-O-siniosperido-5-O-caffeoylquinic acid, belonging to Gardenia jasminoides; one organic acid was identified, chlorogenic acid, shared by Akebia quinata and Citrus reticulata; and one lactone was identified, Atractylodes macrocephala lactone I, belonging to Atractylodes macrocephala.
[0040] The quality detection method of this invention can be used to obtain the presence and characteristics of common characteristic peaks in the chromatogram of the dampness-removing stomach-soothing decoction. This allows for comprehensive monitoring of the quality of the raw materials, semi-finished products, and finished products of the dampness-removing stomach-soothing decoction. By comparing the similarity of chromatographic characteristics, the quality of the dampness-removing stomach-soothing decoction can be evaluated, and its stability and consistency can be examined. This method makes up for the deficiencies of the current quality control methods. At the same time, it can also monitor the stability of the production process of the dampness-removing stomach-soothing decoction, ensuring that its quality is stable, uniform, and controllable.
[0041] The quality testing method of this invention has improved the quality control standards of the finished and semi-finished products of Chushi Weiling Decoction by obtaining the chromatogram of Chushi Weiling Decoction, effectively preventing product counterfeiting and ensuring the normal production and circulation order of Chushi Weiling Decoction. Based on this invention, a correlation study can also be carried out between the chromatogram information detected by liquid chromatography-mass spectrometry and the pharmacodynamic information, thereby further clarifying the correlation between the intrinsic chemical components of Chushi Weiling Decoction and the efficacy of the preparation.
[0042] The quality testing method described in this invention can be used for quality evaluation or control throughout the entire process of research, development, production, and clinical application of the dampness-removing and stomach-strengthening decoction. Attached Figure Description
[0043] Figure 1 These are the UPLC-UV chromatogram and UPLC-TOF-MS total ion chromatogram of the dampness-removing Weiling Decoction in Example 1 of the present invention, wherein from top to bottom are the UPLC-TOF-MS total ion chromatogram (positive ion mode TIC chromatogram), the UPLC-TOF-MS total ion chromatogram (negative ion mode TIC chromatogram) and the UPLC-UV chromatogram of the dampness-removing Weiling Decoction.
[0044] Figure 2 This is a TOF-MS first-order mass spectrum of peaks 1 to 37 of the dampness-removing Weiling Decoction in Example 1 of this invention;
[0045] Figure 3 This is the MS / MS secondary mass spectrum of peaks 1 to 37 of the dampness-removing Weiling Decoction in Example 1 of this invention. Detailed Implementation
[0046] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art can make similar extensions without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0047] Example 1: A quality testing method for a dehumidifying and stomach-strengthening decoction.
[0048] This embodiment uses the dampness-removing Weiling Decoction reference material for quality testing of the decoction. The specific preparation method of the dampness-removing Weiling Decoction reference material is as follows:
[0049] Take one mace each of dried tangerine peel, gardenia, saposhnikovia root, ginger-processed magnolia bark, stir-fried atractylodes rhizome, poria cocos, alisma rhizome, red poria cocos, stir-fried atractylodes rhizome, akebia stem, and talc, three fen each of licorice root and cinnamon bark, two cups of water, add twenty 1.5m pieces of rush pith, decoct until eight-tenths remains, filter, and freeze-dry the resulting decoction to obtain the dry powder of the dampness-removing stomach-strengthening decoction, which is the material basis of the dampness-removing stomach-strengthening decoction.
[0050] This embodiment describes a quality testing method for a dehumidifying and stomach-strengthening decoction, including the following specific steps:
[0051] S1. Preparation of the test solution
[0052] Accurately weigh 2.0g of the dampness-removing Weiling Decoction standard, add 25mL of water, sonicate to dissolve, and pass the entire solution through a D101 macroporous adsorption resin column (inner diameter 1.5cm, column height 12cm). Wash with water until no obvious color is observed, discard the aqueous solution, and then elute with 50mL of 95vol% ethanol aqueous solution. Collect the eluent, evaporate to dryness in a water bath, dissolve the residue in 50vol% methanol aqueous solution, transfer to a 25mL volumetric flask, add 50vol% methanol aqueous solution to the mark, shake well, filter, and obtain the test solution.
[0053] Meanwhile, in the process of preparing the test solution, the concentrated solution of the dampness-removing stomach-soothing decoction can be diluted with water to prepare the dampness-removing stomach-soothing decoction liquid, and then the test solution can be prepared; or, the decoction of the dampness-removing stomach-soothing decoction can be used as the dampness-removing stomach-soothing decoction liquid to prepare the test solution.
[0054] Accurately weigh 5 mL of the concentrated Weiling Decoction for Dehumidification, add 25 mL of water, sonicate to dissolve, and then pass through a D101 macroporous adsorption resin column (inner diameter 1.5 cm, column height 12 cm). Wash with water until no obvious color is observed, discard the aqueous solution, and continue eluting with 50 mL of 95 vol% ethanol aqueous solution. Collect the eluent, evaporate to dryness in a water bath, dissolve the residue in 50 vol% methanol aqueous solution, transfer to a 5 mL volumetric flask, add 50 vol% methanol aqueous solution to the mark, shake well, filter, and obtain the test solution.
[0055] Alternatively, take 25 mL of the decoction for removing dampness and pass it directly through a D101 macroporous adsorption resin column (inner diameter 1.5 cm, column height 12 cm), wash with water until there is no obvious color, discard the water, and continue to elute with 50 mL of 95 vol% ethanol aqueous solution. Collect the eluent, evaporate it to dryness in a water bath, dissolve the residue in 50 vol% methanol aqueous solution, transfer it to a 5 mL volumetric flask, add 50 vol% methanol aqueous solution to the mark, shake well, filter, and obtain the test solution.
[0056] S2, Quality Inspection
[0057] The test solution was subjected to UPLC-Q-TOF-MS detection to obtain the UPLC-UV chromatogram and UPLC-TOF-MS total ion chromatogram (positive and negative ion mode TIC chromatograms) of Chushi Weiling Decoction. This is the chromatogram of Chushi Weiling Decoction. See details below. Figure 1 . Figure 1 The substances in chromatographic peaks 1 to 37 marked in the figure were all well separated and detected.
[0058] The equipment used for UPLC-Q-TOF-MS detection is:
[0059] The Agilent 1290 Infinity II ultra-high performance liquid chromatograph (UPLC) is connected to a G6530C quadrupole-time-of-flight tandem mass spectrometer (Q-TOF-MS) and is equipped with an independent quaternary pump, autosampler, column oven, diode array detector (DAD), and electrospray ionization source (ESI).
[0060] The chromatographic conditions for UPLC-Q-TOF-MS detection are as follows:
[0061] Chromatographic separation was performed using a Waters ACQUITY UPLC HSS T3 C18 UPLC column (2.1 × 100 mm, 1.8 μm) equipped with an online filter; gradient elution was performed using acetonitrile as mobile phase A and 0.1 wt% formic acid aqueous solution as mobile phase B; flow rate was 0.4 mL / min; column temperature was 45℃; detection wavelength was 265 nm; injection volume was 3 μL; the gradient elution conditions were as follows:
[0062] 0–15 min, 8% → 20% mobile phase A, 92% → 80% mobile phase B;
[0063] 15–22 min, 20% → 37% mobile phase A, 80% → 63% mobile phase B;
[0064] 22–27 min, 37% → 70% mobile phase A, 63% → 30% mobile phase B;
[0065] 27–29 min, 70% → 8% mobile phase A, 30% → 92% mobile phase B.
[0066] The mass spectrometry conditions for UPLC-Q-TOF-MS detection were as follows: mass spectrometry was performed in both positive and negative ion modes, with a drying gas temperature of 350℃, a drying gas flow rate of 10 L / min, a nebulizer gas pressure of 35 psi, a sheath gas temperature of 350℃, a sheath gas flow rate of 12 L / min, and capillary voltages of 3500 V (positive mode) and 3500 V (negative mode). The primary mass spectrometry was performed in MS mode with a mass scan range of 100–1200 m / z. The secondary mass spectrometry was performed using Auto MSMS, with the collision voltage adjusted appropriately for different compounds. The obtained LC-MS data were acquired using Agilent MassHunter (B.08.00) software. Data processing was performed using Agilent software QualitativeNavigator (B.08.00) and Qualitative Workflows (B.08.00).
[0067] Furthermore, since talc is a mineral drug, it cannot be analyzed by mass spectrometry.
[0068] By comparing and analyzing the chromatograms of Chushi Weiling Decoction, the medicinal sources of 37 peak substances and the qualitative analysis of the main chromatographic peaks were clarified. Among them, the peaks of the remaining 13 medicinal substances, except for talc, could all be assigned to the chromatograms of Chushi Weiling Decoction.
[0069] First-order mass spectrometry analysis was performed using high-resolution TOF-MS for precise mass number determination, and the results were analyzed... Figure 1 Thirty-seven compounds from peaks 1 to 37 were analyzed and identified. The results are shown in Table 1 and Table 2. Figures 2-3 As shown, these compounds, in positive mode, can generate a molecular ion peak [M+H]. + , and [M+Na] + [M+K] + In isoadductor mode, a molecular ion peak [MH] can be generated; however, in negative mode, a molecular ion peak can be generated. - and [M+Cl] - [M+HCOO] - Isoadduct ions. Based on this information about adduct ions, the precise molecular weight and molecular formula of the compound can be accurately deduced (mass measurement error ≤ 5 ppm, indicating correct matching results), thus aiding in subsequent structural identification.
[0070] The test solution was further analyzed by Auto MS / MS (negative mode predominant) under the same chromatographic conditions, i.e., secondary mass spectrometry analysis, to confirm the structures of some compounds in Table 1. The results are shown in Table 1 and... Figures 2-3 As shown, the results of the first-stage mass spectrometry identification in Table 1 were further confirmed to some extent by the second-stage mass spectrometry analysis.
[0071]
[0072]
[0073]
[0074]
[0075]
[0076]
[0077]
[0078]
[0079]
[0080] In summary, UPLC-QTOF-MS analysis of the test solution prepared from the material reference of Chushi Weiling Decoction detected a total of 37 components. By comparing with literature data and analyzing the accurate molecular weights provided by UPLC-QTOF-MS, these 37 components were identified or inferred, and their medicinal origins were attributed.
[0081] α Flavonoids
[0082] Thirteen flavonoids were identified, namely glucosyl apigenin, glycyrrhizin, apigenin glycyrrhizin, rutin, rutin, hesperidin, styrosinin, isoglycyrrhizin, limonene, glucosyl apigenin, nobiletin, 3,5,6,7,3',4',5'-heptamethoxyflavone, and 5,6,7,8,4'-pentamethoxyflavone, which were attributed to tangerine peel and licorice, respectively.
[0083] β-phenols
[0084] Two phenolic compounds were identified: magnolol and honokiol, both of which are unique to Magnolia officinalis.
[0085] c alkaloids
[0086] Two alkaloid compounds were identified: magnoflorine and magnoflorine, both of which belong to *Magnolia officinalis*.
[0087] d-cyclohexene ethers
[0088] Five iridoid compounds were identified: geniposide B, Jasminoside B, genipin-1-gentiopicoside, geniposide, and ′-O-p-coumaryl quercetin gentiopicoside, all of which belong to Gardenia.
[0089] e-chromogens
[0090] Four chromogens were identified: cimicifugin glycoside, cimicifugin, 5-O-methylvisamidol glycoside, and hyoscyamine glycoside, all of which belong to Saposhnikovia divaricata.
[0091] f saponins
[0092] Two saponin compounds were identified: glycyrrhizin G2 and glycyrrhizic acid, both of which belong to licorice.
[0093] g lignans
[0094] Two lignan compounds were identified, namely magnolinoside B and magnolinoside A, both of which belong to Magnolia officinalis.
[0095] h terpenes
[0096] Three terpenoid compounds were identified: akebia glycoside B, crocin glycoside I, and 16-oxoallotin A, which were attributed to Akebia quinata, Gardenia jasminoides, and Alisma plantago-aquatica, respectively.
[0097] i Organic acid esters
[0098] One organic ester compound was identified as 4-O-sinioyl-5-O-caffeoylquinic acid, which belongs to Gardenia.
[0099] organic acids
[0100] One organic acid compound was identified as chlorogenic acid, which is shared by Akebia quinata and Citrus reticulata peel.
[0101] K lactones
[0102] One lactone compound was identified as atractylone I, which belongs to Atractylodes macrocephala.
[0103] The quality testing method for Chushi Weiling Decoction in this embodiment can be used for quality evaluation or control throughout the entire process of Chushi Weiling Decoction research / development / production / clinical application.
[0104] Examples 2-9: Quality Testing Methods for Dehumidifying Weiling Decoction
[0105] Examples 2-9 are quality testing methods for a dehumidifying stomach-strengthening decoction. Their steps are basically the same as in Example 1, differing only in the process parameters. See Tables 2 and 3 for details.
[0106] Table 2. Summary of process parameters in practical examples 2-5
[0107]
[0108]
[0109] Table 3. Summary of process parameters in Examples 6-9
[0110]
[0111] The process steps and parameters for other parts of Examples 2 to 9 are the same as those in Example 1, and the test results obtained are also similar to those in Example 1, so they will not be repeated here.
[0112] Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.
Claims
1. A method for quality testing of a dehumidifying stomach-strengthening decoction, characterized in that, The quality inspection method includes the following steps: S1. Take the dehumidifying Weiling Decoction liquid and pass it through a macroporous adsorption resin column. Wash with water, discard the water, continue to elute with ethanol aqueous solution, collect the eluent, evaporate to dryness in a water bath, dissolve the residue in methanol aqueous solution, shake well, filter, and prepare the test solution. S2. The quality of the dampness-removing Weiling Decoction was determined by ultra-high performance liquid chromatography-tandem mass spectrometry using the test solution. The mobile phase A for ultra-high performance liquid chromatography detection is acetonitrile, and the mobile phase B is an aqueous solution of formic acid with a concentration of 0.08~0.12wt%. The ultra-high performance liquid chromatography (UHPLC) detection wavelength is 260-270 nm, the column temperature is 40-50 °C, the flow rate is 0.3-0.5 mL / min, and the elution method is gradient elution. The elution conditions for the gradient elution are as follows: 0~15min, 8%→20% mobile phase A, 92%→80% mobile phase B; 15~22 min, 20%→37% mobile phase A, 80%→63% mobile phase B; 22~27 min, 37%→70% mobile phase A, 63%→30% mobile phase B; 27~29 min, 70%→8% mobile phase A, 30%→92% mobile phase B; The quality detection method detected 37 peak substances, namely adenosine, geniposide B, jasminoside B, chlorogenic acid, magnolamine, genipin-1-gentiopicroside, geniposide, magnoflorin B, magnoflorine, glucosylapigenin, magnoflorin A, cimicifugain, glycyrrhizin, apigenin glycyrrhizin, rutin, cimicifugain, akebia ethanol glycoside B, rutin, 5-O-methylvisamidol, hesperidin, 6'-O-p-coumaryl quercetin gentiopicroside, gentiopicroside, and isoglucosinolate. Crocin, 4-O-sinioyl-5-O-caffeoylquinic acid, crocin I, limonin, scutellarin, glucosyl naringin, crocin G2, 16-oxoalisinol A, glycyrrhizic acid, hesperidin, 3,5,6,7,3',4',5'-heptamethoxyflavone, atractylodes lactone I, 5,6,7,8,4'-pentamethoxyflavone, magnolol, and honokiol.
2. The quality testing method for the dehumidifying and stomach-strengthening decoction according to claim 1, characterized in that, The concentration of the ethanol-water solution used for elution is 90-98 vol%, and the volume is 45-60 mL.
3. The quality testing method for the dehumidifying and stomach-strengthening decoction according to claim 1 or 2, characterized in that, The concentration of the methanol-water solution used for dissolution is 40-60 vol.
4. The quality testing method for the dehumidifying and stomach-strengthening decoction according to claim 1 or 2, characterized in that, The liquid form of the dampness-removing Weiling Decoction is made by dissolving the dry powder of the dampness-removing Weiling Decoction in water. Alternatively, it can be prepared by diluting the concentrated Weiling Decoction for Dampness Removal with water. Alternatively, the decoction of Weiling Decoction for Removing Dampness can be used directly as the liquid form of Weiling Decoction for Removing Dampness; When the dry powder of the dehumidifying stomach-soothing decoction is dissolved in water to prepare the liquid dehumidifying stomach-soothing decoction, the weight-to-volume ratio of the dry powder of the dehumidifying stomach-soothing decoction to the prepared test solution is 0.064~0.096g:1mL; When the concentrated dehumidifying Weiling Decoction is diluted with water to prepare the dehumidifying Weiling Decoction liquid, the volume ratio of the concentrated dehumidifying Weiling Decoction to the prepared test solution is 0.8~1.2mL:1mL; When the decoction of Weiling Decoction is used directly as the liquid of Weiling Decoction, the volume ratio of the decoction of Weiling Decoction to the prepared test solution is 4~6mL:1mL.
5. The quality testing method for the dehumidifying and stomach-strengthening decoction according to claim 1 or 2, characterized in that, The mass spectrometry detection was performed in both positive ion mode and negative ion mode.
6. The method for quality testing of the dehumidifying and stomach-strengthening decoction according to claim 1 or 2, characterized in that, The mass spectrometry detection conditions are as follows: drying gas temperature 345~355℃, drying gas flow rate 8~12L / min, nebulizing gas pressure 34~36psi, sheath gas temperature 345~355℃, sheath gas flow rate 11~13L / min, capillary voltage in positive ion mode 3900~4100V, and capillary voltage in negative ion mode 3400~3600V.
7. The method for quality testing of the dehumidifying and stomach-strengthening decoction according to claim 1 or 2, characterized in that, During the mass spectrometry detection process, the first-stage mass spectrometry uses MS mode with a mass scan range of 100~1200 m / z, and the second-stage mass spectrometry uses Auto MSMS.
Citation Information
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