Quality detection method of dampness-eliminating stomach-poria decoction

Using UPLC-Q-TOF-MS technology to detect the quality of Deshi Weiling Decoction solves the problem that existing technology cannot comprehensively monitor the quality of Deshi Weiling Decoction, achieves qualitative analysis and quality control of its chemical components, and ensures product quality stability and consistency.

CN119355153AActive Publication Date: 2025-01-24SHINEWAY PHARMA GRP LTD
View PDF 4 Cites 0 Cited by

Patent Information

Application Number
CN202411366543.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-27
Publication Date
2025-01-24
Estimated Expiration
2044-09-27

AI Technical Summary

Technical Problem

The prior art cannot comprehensively monitor the quality of Deshiweiling Decoction, and especially cannot conduct qualitative analysis of the chemical components contained therein.

Method used

Using ultra-high-efficiency liquid chromatographic spectrals (UPLC-Q-TOF-MS) technology, the quality testing of the test solution of dehumidifying stomach soup is performed. Separation and qualitative analysis of different active ingredients.

Benefits of technology

A accurate analysis of the chemical composition in dehumidification stomach soup has been realized, the source of the medicine flavor of 37 peak substances and the qualitative of the main color spectrum peak can be detected. Stability and consistency.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119355153A_ABST
    Figure CN119355153A_ABST
Patent Text Reader

Abstract

The invention provides a quality detection method of a dampness-eliminating stomach-poria cocos decoction, and belongs to the technical field of medicine detection.The quality detection method comprises the steps that a test solution is prepared firstly, and then the quality of the dampness-eliminating stomach-poria cocos decoction is detected with acetonitrile (A) and 0.08-0.12 wt% formic acid aqueous solution (B) as a mobile phase by means of ultra-high performance liquid chromatography-tandem mass spectrometry. According to the present invention, the UPLC-Q-TOF-MS method is adopted to perform qualitative analysis on the substance-based chemical components of the dampness removing stomach-poria cocos soup, such that the scientific basis is provided for the substance-based material fundamental research of the substance-based material of the dampness removing stomach-poria cocos soup, and the main chemical components of the dampness removing stomach-poria cocos soup are clarified;
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to drug detection technology, in particular to a quality detection method for Chushi Weiling Decoction. Background Art

[0002] Chushi Weiling Decoction, from Volume 4 of "Surgery Authentic", has the effects of clearing away heat and dampness, strengthening the spleen and promoting diuresis. It is mainly used to treat damp-heat congestion in the spleen and lung meridians, which causes fire ulcers and causes pain. Waist fire ulcers (commonly known as snake sores) are damp, with yellow-white color, blisters of varying sizes, ulcers and water, and more pain than dry ones.

[0003] The main ingredients of the Dehumidifying Wei Ling Decoction are tangerine peel, gardenia, saposhnikovia divaricata, ginger and magnolia bark, stir-fried atractylodes, umbellate, oriental Chinese medicine, red tuckahoe, stir-fried white atractylodes, akebia, talcum powder, one qian each, licorice, cinnamon, three fen each, two cups of water, add twenty roots of rush (1.5m), boil for eight fen, and take before meals.

[0004] Ultra-high performance liquid chromatography tandem mass spectrometry has high analysis efficiency and speed, can obtain accurate molecular structure information, can obtain primary and multi-level mass spectrometry information of each compound, and provides a good technical means for multi-index component analysis of complex Chinese medicine systems. Dehumidification Weiling Decoction is made of 14 Chinese medicines, and its ingredients are extremely complex. At present, it is impossible to comprehensively monitor the quality of Dehumidification Weiling Decoction, let alone conduct qualitative analysis of the chemical components contained in Dehumidification Weiling Decoction. Therefore, it is necessary to develop a quality detection method for Dehumidification Weiling Decoction, so as to more comprehensively evaluate the quality of Dehumidification Weiling Decoction. Summary of the invention

[0005] In view of the above problems, the present invention provides a quality detection method for Chushi Weiling Decoction.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is:

[0007] A quality detection method for Chushi Weiling Decoction, the quality detection method comprising the following steps:

[0008] S1. Prepare the test solution with Chushi Weiling Decoction;

[0009] S2. Take the test solution and use ultra-high performance liquid chromatography tandem mass spectrometry to detect the quality of Chushi Weiling Decoction;

[0010] The mobile phase A of the ultra-high performance liquid chromatography detection is acetonitrile, and the mobile phase B is a formic acid aqueous solution with a concentration of 0.08-0.12 wt%;

[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] 27-29min, 70%→8% mobile phase A, 30%→92% mobile phase B.

[0017] Furthermore, the test solution is prepared by passing the dehumidified Wei Ling decoction liquid through a macroporous adsorption resin column, washing with water, discarding the water, and continuously eluting with an ethanol aqueous solution, collecting the eluate, evaporating it in a water bath, dissolving the residue with a methanol aqueous solution, shaking well, and filtering.

[0018] Furthermore, the concentration of the ethanol aqueous solution used for elution is 90 to 98 vol%, and the amount used is 45 to 60 mL.

[0019] Furthermore, the concentration of the methanol aqueous solution used for dissolution is 40 to 60 vol%.

[0020] Furthermore, the dehumidifying Wei Ling Tang liquid is prepared by dissolving the dehumidifying Wei Ling Tang dry paste powder in water;

[0021] Alternatively, it can be prepared by diluting the concentrated solution of Chushi Weiling Decoction with water;

[0022] Alternatively, the decoction of Chushi Weiling Decoction is directly used as the liquid of Chushi Weiling Decoction;

[0023] When the dehumidified Weiling decoction dry paste powder is dissolved in water to prepare the dehumidified Weiling decoction liquid, the weight volume ratio of the dehumidified Weiling decoction dry paste powder to the prepared test solution is 0.064-0.096 g:1 mL;

[0024] When the Dehumidification Weiling Decoction concentrate is diluted with water to prepare the Dehumidification Weiling Decoction liquid, the volume ratio of the Dehumidification Weiling Decoction concentrate to the prepared test solution is 0.8-1.2 mL:1 mL;

[0025] When the Chushi Weiling Decoction decoction is used directly as the Chushi Weiling Decoction liquid, the volume ratio of the Chushi Weiling Decoction decoction to the prepared test sample solution is 4-6 mL:1 mL.

[0026] Furthermore, the mass spectrometry detection is performed in positive ion mode and negative ion mode respectively.

[0027] Furthermore, the conditions for mass spectrometry detection are: 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, in the mass spectrometry detection process, the primary mass spectrometry adopts MS mode with a mass scanning range of 100 to 1200 m / z, and the secondary mass spectrometry adopts Auto MSMS.

[0029] Furthermore, the detection wavelength of the ultra-high performance liquid chromatography is 260-270 nm.

[0030] Furthermore, the column temperature of the ultra-high performance liquid chromatography is 40-50° C. and the flow rate is 0.3-0.5 mL / min.

[0031] The beneficial effects of the quality detection method of the Dehumidifying Weiling Decoction of the present invention are:

[0032] The present invention adopts UPLC-Q-TOF-MS method to qualitatively analyze the chemical components of the Chushi Weiling Decoction material benchmark, provides a scientific basis for the material basis research of the Chushi Weiling Decoction material benchmark, and clarifies its main chemical composition;

[0033] The present invention adopts UPLC-Q-TOF-MS method to qualitatively analyze the chemical components of the Chushi Weiling Decoction reference material, which has high analysis efficiency and fast speed, can obtain accurate molecular structure information in the Chushi Weiling Decoction, can obtain primary and multi-level mass spectrum information of each compound, and provides a good technical means for multi-index component analysis of complex traditional Chinese medicine system such as Chushi Weiling Decoction.

[0034] The present invention adopts UPLC-Q-TOF-MS method to qualitatively analyze the chemical components of the reference substance of Chushi Weiling Decoction, provides a scientific basis for the material basis research of Chushi Weiling Decoction, and clarifies its main chemical composition;

[0035] The quality detection method of the present invention can detect almost all the medicinal ingredients in the whole recipe of Chushi Weiling Decoction;

[0036] The present invention achieves the purpose of separating the different effective components in the Chushi Weiling Decoction well by changing the elution system and utilizing the different physical and chemical properties of the different effective components in the Chushi Weiling Decoction to change the chromatographic conditions.

[0037] The present invention can obtain a spectrum of Chushi Weiling Decoction with better peaks by selecting specific chromatographic conditions and mass spectrometry conditions.

[0038] The quality detection method of the present invention also has good feasibility, stability and reproducibility;

[0039] The quality detection method of the present invention can detect and clarify the medicinal taste sources of 37 peak substances and the qualitative identification of the main chromatographic peaks; among them, a total of 13 flavonoid compounds are identified, namely, glucosyl apigenin, liquiritin, apiosyl liquiritin, rutin, rutin, hesperidin, formononetin, isoliquiritigenin, citrus glycosides, glucosyl naringin, nobiletin, 3,5,6,7,3',4',5'-heptamethoxyflavone, 5,6,7,8,4'-pentamethoxyflavone, which belong to dried orange peel and licorice respectively; a total of 2 phenolic compounds are identified, namely, honokiol and magnolol, which are both unique components of ginger magnolia bark; a total of 2 alkaloid compounds are identified, namely, magnoflorine and Magnoflorine, which are both belonging to ginger magnolia bark; a total of 5 iridoid terpenoid compounds are identified, namely, jasminoside B, jasminoside B, genipin-1-gentiobioside, gardenia glycoside, ′-O-p-coumaroylquercetin gentiobioside, all belong to Gardenia jasminoides; a total of 4 chromone compounds were identified, namely, cimicifuga glycoside, cimicifuga glycoside, 5-O-methylvisaminol glycoside, and chamoyl glycoside, all belong to Saposhnikovia divaricata; a total of 2 saponin compounds were identified, namely, glycyrrhizin G2 and glycyrrhizic acid, all belong to Glycyrrhiza uralensis; a total of 2 lignan compounds were identified, namely, magnolin B and magnolin A total of 3 terpenoid compounds were identified, namely, edible ethanol glycoside B, crocin I, and 16-oxo alismatol A, which were respectively attributed to edible, gardenia, and oriental water chestnuts; a total of 1 organic acid ester compound was identified as 4-O-sinapoyl-5-O-caffeoylquinic acid, which was attributed to gardenia; a total of 1 organic acid compound was identified as chlorogenic acid, which was shared by edible and dried orange peel; a total of 1 lactone compound was identified as atractylodes lactone I, which was attributed to Atractylodes macrocephala;

[0040] By using the quality detection method of the present invention, the presence and characteristics of the characteristic peaks in the spectrum of the obtained Dehumidification Weiling Decoction can be obtained, and the quality of the raw medicinal materials, semi-finished products and finished products of the Dehumidification Weiling Decoction can be comprehensively monitored. By comparing the similarity of the chromatographic characteristics, the quality of the Dehumidification Weiling Decoction can be evaluated, and the stability and consistency can be examined, which makes up for the shortcomings of the current quality control method. At the same time, the stability of the production process of the Dehumidification Weiling Decoction can also be monitored to ensure that its quality is stable, uniform and controllable.

[0041] By utilizing the quality inspection method of the present invention, the spectrum of Chushi Weiling Decoction obtained improves the quality monitoring standards of the finished and semi-finished products of Chushi Weiling Decoction, effectively prevents the occurrence of product counterfeiting incidents, and ensures the normal production and circulation order of Chushi Weiling Decoction; on the basis of the present invention, a study on the correlation between the spectrum information detected by liquid chromatography-mass spectrometry and the pharmacodynamic activity information can also be carried out, thereby deeply clarifying the correlation between the intrinsic chemical components of Chushi Weiling Decoction and the efficacy of the preparation.

[0042] The quality detection method of the present invention can be used for quality evaluation or control of the entire process of research / development / production / clinical application of Chushi Weiling Decoction. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 It is the UPLC-UV chromatogram and the UPLC-TOF-MS total ion current diagram of the Dehumidification Weiling Decoction in Example 1 of the present invention, wherein from top to bottom are the UPLC-TOF-MS total ion current diagram (positive ion mode TIC diagram), the UPLC-TOF-MS total ion current diagram (negative ion mode TIC diagram) and the UPLC-UV chromatogram of the Dehumidification Weiling Decoction;

[0044] Figure 2 It is a TOF-MS primary mass spectrum of peak substances No. 1 to No. 37 of the Chushi Weiling Decoction in Example 1 of the present invention;

[0045] Figure 3 It is the MS / MS secondary mass spectrum of peak substances No. 1 to 37 of the Chushi Weiling Decoction in Example 1 of the present invention. DETAILED DESCRIPTION

[0046] The technical solutions in the embodiments of the present invention are described clearly and completely below. In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention can also be implemented in other ways different from those described herein, and those skilled in the art can make similar generalizations without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below.

[0047] Embodiment 1 A kind of quality detection method of dehumidification Weiling decoction

[0048] This embodiment uses the Dehumidifying Weiling Decoction reference material to perform quality detection of the Dehumidifying Weiling Decoction. The specific preparation method of the Dehumidifying Weiling Decoction reference material is as follows:

[0049] Take one qian each of dried tangerine peel, gardenia, siler, ginger magnolia bark, stir-fried atractylodes, umbellate, oriental medicine, red tuckahoe, stir-fried atractylodes, akebia, talcum powder, three fen each of licorice and cinnamon, two cups of water, add twenty roots of rush (1.5m), boil for eight minutes, filter, and the decoction obtained is freeze-dried to obtain the dry paste powder of Dehumidifying Weiling Decoction, which is the material standard of Dehumidifying Weiling Decoction.

[0050] The present embodiment is a quality detection method of a dehumidifying Weiling decoction, comprising the following specific steps:

[0051] S1. Preparation of test solution

[0052] Take 2.0 g of the standard substance of Dehumidification Weiling Decoction, accurately weigh it, add 25 mL of water, dissolve it with ultrasound, and pass it all through a D101 macroporous adsorption resin column (inner diameter 1.5 cm, column height 12 cm), wash it with water until there is no obvious color, discard the water, and then elute it with 50 mL of 95 vol% ethanol aqueous solution, collect the eluate, evaporate it in a water bath, dissolve the residue in 50 vol% methanol aqueous solution, transfer it to a 25 mL volumetric flask, add 50 vol% methanol aqueous solution to the scale, shake well, filter, and obtain the test solution.

[0053] Meanwhile, in the process of preparing the test solution, the Dehumidification Weiling Decoction concentrate can be diluted with water to prepare the Dehumidification Weiling Decoction liquid to prepare the test solution; or, the Dehumidification Weiling Decoction decoction can be used as the Dehumidification Weiling Decoction liquid to prepare the test solution.

[0054] That is, take 5mL of Dehumidification Weiling Decoction concentrate and accurately weigh it, add 25mL of water, dissolve it by ultrasonic treatment, and then pass it through a D101 macroporous adsorption resin column (inner diameter 1.5cm, column height 12cm), wash it with water until there is no obvious color, discard the water, continue to elute with 50mL of 95vol% ethanol aqueous solution, collect the eluate, evaporate it in a water bath, dissolve the residue in 50vol% methanol aqueous solution, transfer it to a 5mL volumetric flask, add 50vol% methanol aqueous solution to the scale, shake well, filter, and prepare the test solution.

[0055] Alternatively, take 25 mL of the decoction of Chushi Weiling Decoction and directly pass it 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, continue to elute with 50 mL of 95 vol% ethanol aqueous solution, collect the eluate, evaporate to dryness in a water bath, add 50 vol% methanol aqueous solution to dissolve the residue, transfer it to a 5 mL volumetric flask, add 50 vol% methanol aqueous solution to the scale, shake well, filter, and prepare 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 current diagram (positive and negative ion mode TIC diagram) of Chushi Weiling Decoction, which is the spectrum of Chushi Weiling Decoction. Figure 1 . Figure 1 The chromatographic peak substances No. 1 to 37 marked in the figure were all well separated and detected.

[0058] Among them, the equipment used for UPLC-Q-TOF-MS detection is:

[0059] Agilent 1290 Infinity II ultra-high performance liquid chromatograph (UPLC) was connected to a G6530C quadrupole-time-of-flight tandem mass spectrometer (Q-TOF-MS) 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:

[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; acetonitrile was used as mobile phase A, and 0.1 wt % formic acid aqueous solution was used as mobile phase B for gradient elution; flow rate was 0.4 mL / min; column temperature was 45° C.; detection wavelength was 265 nm; injection volume was 3 μ L; the elution conditions for gradient elution were:

[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] 27-29min, 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 detection was performed in positive and negative ion modes, respectively, with a drying gas temperature of 350°C, a drying gas flow rate of 10 L / min, a nebulizer gas pressure of 35 psi, a sheath gas temperature of 350°C, a sheath gas flow rate of 12 L / min, and a capillary voltage of 3500 V (positive mode) and 3500 V (negative mode). The primary mass spectrometry used the MS mode with a mass scanning range of 100-1200 m / z. The secondary mass spectrometry used Auto MSMS, and the collision voltage was appropriately adjusted according to different compounds. The obtained LC-MS data were collected by Agilent MassHunter (B.08.00) software. Data processing used 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 spectrum of Chushi Weiling Decoction, the origins of 37 peak substances and the qualitative identification of the main chromatographic peaks were clarified. Among them, the peaks of the spectrum of Chushi Weiling Decoction can be obtained for the remaining 13 ingredients except talc.

[0069] The accurate mass number of high-resolution TOF-MS was used to measure the mass of the Figure 1 The 37 compounds in peaks 1 to 37 were analyzed and identified. The results are shown in Table 1 and Figure 2-Figure 3 As shown. It can be seen that these compounds can generate molecular ion peaks [M+H] in positive mode. + , and [M+Na] + , [M+K] + In negative mode, molecular ion peaks [MH] are generated. - and [M+Cl] - 、[M+HCOO] - Based on the information of these adduct ions, the precise molecular weight and molecular formula of the compound can be accurately inferred (the mass measurement error is ≤5ppm, indicating that the matching result is correct), which is helpful for its subsequent structural identification.

[0070] The test solution was further subjected to Auto MS / MS analysis (mainly in negative mode) under the same chromatographic conditions, that is, secondary mass spectrometry analysis was performed to confirm the structures of some of the compounds in Table 1. The results are shown in Tables 1 and Figure 2-Figure 3 The secondary mass spectrometry analysis further confirmed the primary mass spectrometry identification results in Table 1 to a certain extent.

[0071]

[0072]

[0073]

[0074]

[0075]

[0076]

[0077]

[0078]

[0079]

[0080] In summary, UPLC-QTOF-MS analysis of the test solution prepared based on the Chushi Weiling Decoction material standard detected 37 components in total. By comparing with literature data and analyzing the accurate molecular weight given by UPLC-QTOF-MS, a total of 37 components were identified or speculated, and the source of the compounds was attributed.

[0081] aFlavone

[0082] A total of 13 flavonoids were identified, including glucosyl apigenin, liquiritin, apiosyl liquiritin, rutin, naringin, hesperidin, formononetin, isoliquiritigenin, citrus glycoside, glucosyl naringin, nobiletin, 3,5,6,7,3',4',5'-heptamethoxyflavone and 5,6,7,8,4'-pentamethoxyflavone, which belong to tangerine peel and licorice, respectively.

[0083] b phenols

[0084] A total of two phenolic compounds were identified, namely honokiol and magnolol, both of which are unique components of Zingiber officinale.

[0085] c Alkaloids

[0086] A total of two alkaloid compounds were identified, namely magnoflorine and magnoflorine, both of which belong to Magnolia officinalis.

[0087] d-Iridoids

[0088] A total of five iridoid ether terpenoid compounds were identified, namely, jasminoside B, jasminoside B, genipin-1-gentiobioside, gardenoside, and ′-O-p-coumaroylquercetin gentiobioside, all of which belong to Gardenia jasminoides.

[0089] E-chromones

[0090] A total of four chromone compounds were identified, namely, cimicifuga glycoside, cimicifuga glycoside, 5-O-methylvisaminol glycoside, and chamoyl glycoside, all of which belong to Saposhnikovia divaricata.

[0091] fSaponins

[0092] A total of two saponin compounds were identified, namely glycyrrhizin G2 and glycyrrhizic acid, both of which belong to licorice.

[0093] g Lignans

[0094] A total of two lignan compounds were identified, namely magnolin B and magnolin A, both belonging to Magnolia officinalis.

[0095] h terpenes

[0096] A total of three terpenoid compounds were identified, namely, Akebia ethanoloside B, Crocin I, and 16-oxoalismol A, which belonged to Akebia, Gardenia, and Alisma orientalis, respectively.

[0097] iOrganic acid esters

[0098] One organic acid ester compound was identified as 4-O-sinapoyl-5-O-caffeoylquinic acid, which belongs to Gardenia jasminoides.

[0099] jOrganic acids

[0100] A total of one organic acid compound was identified as chlorogenic acid, which is shared by Akebia and Citrus reticulata.

[0101] k-lactones

[0102] A total of one lactone compound was identified as atractylodes lactone I, which belongs to Atractylodes macrocephala.

[0103] The quality detection method of the Dehumidification Weiling Decoction in this embodiment can be used for quality evaluation or control of the entire process of research / development / production / clinical application of the Dehumidification Weiling Decoction.

[0104] Embodiment 2~9 the quality detection method of dehumidification Weiling decoction

[0105] Examples 2 to 9 are respectively a method for detecting the quality of Dehumidifying Weiling Decoction, and their steps are substantially the same as those of Example 1, except that the only difference is the different process parameters, as shown in Tables 2 and 3:

[0106] Table 2 List of process parameters in Examples 2 to 5

[0107]

[0108]

[0109] Table 3 List of process parameters in Examples 6 to 9

[0110]

[0111] The process steps and parameters of other parts of Examples 2 to 9 are the same as those of Example 1, and the obtained test results are also similar to those of Example 1, which will not be repeated here.

[0112] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

Claims

1. A quality detection method for Chushi Weiling Decoction, characterized in that: The quality detection method comprises the following steps: S1. Prepare the test solution with Chushi Weiling Decoction; S2. Take the test solution and use ultra-high performance liquid chromatography tandem mass spectrometry to detect the quality of Chushi Weiling Decoction; The mobile phase A of the ultra-high performance liquid chromatography detection is acetonitrile, and the mobile phase B is a formic acid aqueous solution with a concentration of 0.08-0.12wt%; The elution mode of the ultra-high performance liquid chromatography detection is gradient elution; The elution conditions of the gradient elution are: 0-15 min, 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; 27~29min, 70%→8% mobile phase A, 30%→92% mobile phase B.

2. The quality detection method of Chushi Weiling Decoction according to claim 1, characterized in that: The test solution is prepared by passing the dehumidified Wei Ling decoction liquid through a macroporous adsorption resin column, washing with water, discarding the water, eluting with an ethanol aqueous solution, collecting the eluate, evaporating it in a water bath, dissolving the residue with a methanol aqueous solution, shaking well, and filtering.

3. The quality detection method of Dehumidifying Weiling Decoction according to claim 2, characterized in that: The concentration of the ethanol aqueous solution used for elution is 90-98 vol%, and the amount used is 45-60 mL.

4. The quality detection method of Dehumidifying Weiling Decoction according to claim 2 or 3, characterized in that: The concentration of the methanol aqueous solution used for dissolution is 40 to 60 vol%.

5. The quality detection method of Dehumidifying Weiling Decoction according to claim 2 or 3, characterized in that: The liquid of Chushi Weiling Decoction is prepared by dissolving the dry powder of Chushi Weiling Decoction in water; Alternatively, it can be prepared by diluting the concentrated solution of Chushi Weiling Decoction with water; Alternatively, the decoction of Chushi Weiling Decoction is directly used as the liquid of Chushi Weiling Decoction; When the dehumidified Weiling Decoction dry paste powder is dissolved in water to prepare the dehumidified Weiling Decoction liquid, the weight volume ratio of the dehumidified Weiling Decoction dry paste powder to the prepared test solution is 0.064-0.096 g:1 mL; When the Dehumidification Weiling Decoction concentrate is diluted with water to prepare the Dehumidification Weiling Decoction liquid, the volume ratio of the Dehumidification Weiling Decoction concentrate to the prepared test solution is 0.8~1.2mL:1mL; When the Chushi Weiling Decoction decoction is used directly as the Chushi Weiling Decoction liquid, the volume ratio of the Chushi Weiling Decoction decoction to the prepared test sample solution is 4~6mL:1mL.

6. The quality detection method of Chushi Weiling Decoction according to any one of claims 1 to 3, characterized in that: The mass spectrometry detection is performed in positive ion mode and negative ion mode respectively.

7. The quality detection method of Chushi Weiling Decoction according to any one of claims 1 to 3, characterized in that: The conditions for mass spectrometry detection are: drying gas temperature 345~355°C, drying gas flow rate 8~12L / min, nebulizing gas pressure 34~36psi, sheath gas temperature 345~355°C, sheath gas flow rate 11~13L / min, capillary voltage in positive ion mode is 3900~4100V, and capillary voltage in negative ion mode is 3400~3600V.

8. The quality detection method of Chushi Weiling Decoction according to any one of claims 1 to 3, characterized in that: In the mass spectrometry detection process, the primary mass spectrometry adopts MS mode with a mass scanning range of 100-1200 m / z, and the secondary mass spectrometry adopts AutoMSMS.

9. The quality detection method of Chushi Weiling Decoction according to any one of claims 1 to 3, characterized in that: The detection wavelength of the ultra-high performance liquid chromatography is 260-270 nm.

10. The quality detection method of Chushi Weiling Decoction according to any one of claims 1 to 3, characterized in that: The column temperature of the ultra-high performance liquid chromatography is 40-50° C. and the flow rate is 0.3-0.5 mL / min.

Citation Information

Patent Citations

  • Application of triterpene from poria cocos peel in preparation of medicines for treating nephropathy

    CN106974917A

  • Traditional Chinese medicine composition for treating eczema and preparing method and application

    CN107184860A

  • Construction method and application of fingerprint spectrum of Huopingxiaolingling decoction

    CN116519825A

  • Method for simultaneously extracting polysaccharides and triterpenes in poria cocos

    CN117736350A