Quality control method of traditional Chinese medicine compound for gastric ulcer

Abstract

The invention provides a quality control method of a traditional Chinese medicine compound for gastric ulcer. The method comprises the following steps: using a calycosin reference substance, an isoliquiritigenin reference substance, a ceratin reference substance, a formononetin reference substance, a parthenolide reference substance, an atractylenolide I reference substance, an atractylenolide II reference substance, an isohesperidin reference substance, a tyrosine reference substance, an atractylenolide III reference substance and a cryptochlorogenic acid reference substance; and preparing a mixed reference substance solution from the honeysuckle glycoside reference substance, and determining the contents of the 12 components in the traditional Chinese medicine solution to be tested. The invention establishes a traditional Chinese medicine compound quality control method for gastric ulcer, and the method can be applied to quality control of a Chinese patent medicine monkshood middle-jiao-regulating pill.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine component determination technology, specifically relating to a quality control method for traditional Chinese medicine compound prescriptions used for gastric ulcers. Background Technology

[0002] Pathological studies have shown that the traditional Chinese medicine compound "Fuzi Lizhong Decoction" has a therapeutic effect on gastric ulcers. However, due to the complex chemical composition of traditional Chinese medicine compound formulas, the different sources of medicinal materials, and the large differences in the content of the main components, the quality of the finished product is easily unstable, affecting its efficacy. Summary of the Invention

[0003] The technical problem to be solved by the present invention is to provide a quality control method for traditional Chinese medicine compound formulas for gastric ulcers, which addresses the shortcomings of the prior art. This quality control method for traditional Chinese medicine compound formulas for gastric ulcers can be applied to the quality control of the traditional Chinese medicine preparation Fuzi Lizhong Wan.

[0004] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: a quality control method for a traditional Chinese medicine compound for gastric ulcers, the method being as follows: S1. Preparation of mixed reference solution: Weigh out the reference standards for verbascoside, isoglycyrrhizin, cheronitrile, styroside, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohexadecanol, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside, respectively, and dilute to volume with anhydrous ethanol to obtain 12 reference solutions. Take equal volumes of each reference solution, mix them, and dilute to volume with anhydrous ethanol to obtain a mixed reference solution; S2. Preparation of the test Chinese herbal medicine solution: The traditional Chinese medicine for gastric ulcers was soaked in distilled water, extracted twice by reflux, and the two extracts were combined, filtered through gauze, concentrated in a rotary evaporator at 70°C, centrifuged, evaporated to dryness at 70°C, dissolved in anhydrous ethanol by ultrasonication, and brought to a final volume to obtain the test traditional Chinese medicine solution; the traditional Chinese medicine for gastric ulcers consisted of equal masses of Aconitum carmichaelii, Codonopsis pilosula, Zingiber officinale, Glycyrrhiza uralensis, and Atractylodes macrocephala. S3, Measurement: The mixed reference solution obtained in S1 and the test traditional Chinese medicine solution obtained in S2 were injected under the following liquid chromatography-tandem mass spectrometry conditions: S301, Liquid Chromatography Conditions: A 50 mm × 2.1 mm Hypersil Gold column with a particle size of 1.9 μm was used; the column temperature was 30 °C; the mobile phase was methanol + water; the gradient elution conditions were: 0–6 min, methanol volume ratio of mobile phase 25%–80%; 6 min–7 min, methanol volume ratio of mobile phase 80%–95%; 7 min–8 min, methanol volume ratio of mobile phase 95%–100%; 8 min–9 min, methanol volume ratio of mobile phase 100%; the flow rate was 0.3 mL / min. S302, Mass Spectrometry Conditions: Scanning mode: Full-MS / DD-MS2, simultaneous acquisition of positive and negative ions; positive ion scanning range 100 m / z~1500 m / z, negative ion scanning range 100 m / z~1500 m / z; resolution 17500; capillary temperature: 300℃; spray voltage: 4.0 kV and -3.5 kV; sheath gas volumetric flow rate 35 L / h; S-lens voltage 50 V; S4, Judgment: A blank solvent was set as a control. Under the conditions of liquid chromatography described in S301 and mass spectrometry described in S302, the presence of corresponding chemical components in the tested Chinese medicine solution was determined based on the chromatographic retention time and the precise molecular weight of the mass spectrometer. The mixed reference solution obtained in S1 was diluted into 5 mass concentration gradients. The mass concentration of each chemical component was plotted on the x-axis and the peak area on the y-axis. Standard working curves for 12 chemical components were plotted. The tested Chinese medicine solution obtained in S2 was quantified using the standard working curves. The response values ​​of the chemical components in the tested Chinese medicine solution were within the linear range of the instrument detection. The method for determining whether the corresponding chemical components exist in the tested traditional Chinese medicine solution is as follows: the chromatographic retention time and precise molecular weight information of the chemical components in the tested traditional Chinese medicine solution should be consistent with the information of the corresponding components in the mixed reference solution, with an allowable deviation of less than ±2.5%. The linear equation for verbascoside isoflavone is y = 1 × 10 12 x+1×10 7 r 2 =0.9951, with a linear range of 0.0032~0.16 μg / mL; The linear equation for isoliquiritigenin is y = 9 × 10 11 x + 7 × 10 6 r 2 =0.9965, with a linear range of 0.0032~0.16 μg / mL; The linear equation for saflavin is y = 8 × 10 10 x+236293, r 2=0.9966, with a linear range of 0.0016~0.08 μg / mL; The linear equation for styracin is y = 5 × 10 11 x + 4 × 10 6 r 2 =0.9967, with a linear range of 0.0032~0.16 μg / mL; The linear equation for ternolactone is y = 1 × 10 11 x+867278, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone I is y = 6 × 10 11 x + 4 × 10 6 r 2 =0.9988, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone II is y = 9 × 10 11 x + 6 × 10 6 r 2 =0.9959, with a linear range of 0.0032~0.16 μg / mL; The linear equation for isohesperidin is y = 1 × 10 12 x+8×10 6 r 2 =0.9953, with a linear range of 0.0016~0.08 μg / mL; The linear equation for tyrosine is y = 4 × 10 10 x+846033, r 2 =0.9960, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone III is y = 1 × 10 10 x+36813, r 2 =0.9955, with a linear range of 0.0032~0.16 μg / mL; The linear equation for cryptochlorogenic acid is y = 1 × 10 11 x-173653, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The linear equation for lycopene is y = 8 × 10 10 x+52376, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The contents of the chemical components contained in the traditional Chinese medicine were determined as follows: verbascoside, isoliquiritin, saflavin, styroside, chrysanthemum flavonoid, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside.

[0005] Preferably, in S2, the first reflux extraction is performed for 30 minutes, and the second reflux extraction is performed for 20 minutes.

[0006] Preferably, the ratio of the traditional Chinese medicine for gastric ulcers to distilled water in S2 is 1g:10mL.

[0007] Preferably, the soaking time in S2 is 30 minutes.

[0008] Preferably, the ultrasonic dissolution time in S2 is 5 minutes.

[0009] Preferably, the centrifugation conditions in S2 are: 4℃, 10000rpm, 10min.

[0010] Compared with the prior art, the present invention has the following advantages: This invention establishes a quality control method for traditional Chinese medicine compound formulas for gastric ulcers, which can be applied to the quality control of the traditional Chinese medicine Fuzi Lizhong Wan.

[0011] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments. Attached Figure Description

[0012] Figure 1 This is the extraction ion chromatogram of verbascoside, isoliquiritigenin, cheriflavin, gentianin, chrysanthemum flavonoid, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside extracted using anhydrous ethanol blank reagent in Example 1 of the present invention.

[0013] Figure 2 This is the extraction ion chromatogram of verbascoside, isoglycyrrhizin, cheriflavin, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside extracted from the mixed reference solution of Example 1 of the present invention. Detailed Implementation

[0014] Example 1 A quality control method for a traditional Chinese medicine compound used for gastric ulcers, the method being as follows: S1. Preparation of mixed reference solution: Weigh out 2.0 mg each of the following reference standards: verbascoside, isoliquiritin, 1.0 mg of safflower flavonoid, 2.0 mg of gentianin, 2.0 mg of ternolactone, 2.0 mg of atractylodes lactone I, 2.0 mg of atractylodes lactone II, 1.0 mg of isohesperidin, 2.0 mg of tyrosine, 2.0 mg of atractylodes lactone III, 2.0 mg of cryptochlorogenic acid, and 2.0 mg of lycopene. Add anhydrous ethanol to each standard and bring the volume to 5 ml. Twelve reference solutions were obtained in mL volumetric flasks, namely, verbascoside reference solution, isoglycyrrhizin reference solution, cheronitin reference solution, styrosine reference solution, baicalein reference solution, baicalein reference solution, atractylodes lactone reference solution, atractylodes lactone I reference solution, atractylodes lactone II reference solution, isohexolone reference solution, tyrosine reference solution, atractylodes lactone III reference solution, cryptochlorogenic acid reference solution, and honeysuckle glycoside reference solution; Take 400 μL of each reference solution separately, mix them, and dilute to 10 mL in a volumetric flask with anhydrous ethanol to obtain a mixed reference solution; S2. Preparation of the test Chinese herbal medicine solution: The traditional Chinese medicine for gastric ulcers (1 g Aconitum carmichaelii, 1 g Codonopsis pilosula, 1 g dried ginger, 1 g licorice, and 1 g Atractylodes macrocephala) was soaked in distilled water at a ratio of 1 g: 10 mL for 30 min to ensure complete wetting. The mixture was then subjected to two reflux extractions: the first for 30 min and the second for 20 min. The extracts were combined, filtered through gauze, concentrated in a rotary evaporator at 70 °C, centrifuged at 10000 rpm for 10 min at 4 °C, evaporated to dryness at 70 °C, dissolved in anhydrous ethanol by sonication for 5 min, and diluted to a 10 mL volumetric flask to obtain the test herbal solution (Fuzi Lizhong Decoction). S3, Measurement: The mixed reference solution obtained in S1 and the test traditional Chinese medicine solution obtained in S2 were injected under the following conditions set for liquid chromatography-tandem mass spectrometry (UHPLC-MS detection): S301, Liquid Chromatography Conditions: A 50 mm × 2.1 mm Hypersil Gold column with a particle size of 1.9 μm was used; the column temperature was 30 °C; the mobile phase was methanol + water; the gradient elution conditions were: 0–6 min, methanol volume ratio of mobile phase 25%–80%; 6 min–7 min, methanol volume ratio of mobile phase 80%–95%; 7 min–8 min, methanol volume ratio of mobile phase 95%–100%; 8 min–9 min, methanol volume ratio of mobile phase 100%; the flow rate was 0.3 mL / min. S302, Mass Spectrometry Conditions: Scanning mode: Full-MS / DD-MS2, simultaneous acquisition of positive and negative ions; positive ion scanning range 100 m / z~1500 m / z, negative ion scanning range 100 m / z~1500 m / z; resolution 17500; capillary temperature: 300℃; spray voltage: 4.0 kV and -3.5 kV; sheath gas volumetric flow rate 35 L / h; S-lens voltage 50 V; S4, Judgment: A blank solvent was set as a control. Under the conditions of liquid chromatography described in S301 and mass spectrometry described in S302, the presence of corresponding chemical components in the tested Chinese medicine solution was determined based on the chromatographic retention time and the precise molecular weight of the mass spectrometer. The mixed reference solution obtained in S1 was diluted into 5 mass concentration gradients. The mass concentration of each chemical component was plotted on the x-axis and the peak area on the y-axis. Standard working curves for 12 chemical components were plotted. The tested Chinese medicine solution obtained in S2 was quantified using the standard working curves. The response values ​​of the chemical components in the tested Chinese medicine solution were within the linear range of the instrument detection. The method for determining whether the corresponding chemical components exist in the tested traditional Chinese medicine solution is as follows: the chromatographic retention time and precise molecular weight information of the chemical components in the tested traditional Chinese medicine solution should be consistent with the information of the corresponding components in the mixed reference solution, with an allowable deviation of less than ±2.5%. The contents of the chemical components contained in the traditional Chinese medicine were determined as follows: verbascoside, isoliquiritin, saflavin, styroside, chrysanthemum flavonoid, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside.

[0015] Methodological investigation (1) Systematic investigation: The systematic investigation is to investigate whether there are chromatographic peaks in the anhydrous ethanol reagent that interfere with these 12 chemical components. First, the anhydrous ethanol and the mixed reference solution were filtered through a 0.22 μm microporous membrane and then detected by liquid chromatography-mass spectrometry.

[0016] (2) Examination of linear relationship: The examination of linear relationship uses the peak area as the ordinate (Y) and the concentration of each reference standard as the abscissa (X). The linear regression equation is calculated, and r is used as the expression. 2 >0.995 was used as the criterion for good linearity. First, the mixed reference solution was serially diluted by 10, 20, 50, 100, 200, 500, 1000, 2000, and 5000 times to prepare mixed reference solutions with 9 concentration gradients. All solutions were then filtered through a 0.22 μm microporous membrane and detected according to the conditions in step S3.

[0017] (3) Precision test: The precision test is based on RSD≤3% as the standard for good precision. After taking the mixed reference solution diluted 20 times, filter it through a 0.22 μm microporous membrane and inject it 6 times in a row, 2 μL each time. Calculate the RSD value of the peak area of ​​the Target-SIM extracted ion chromatogram of each reference in the 6 injections.

[0018] (4) Stability test: The stability test was based on RSD ≤ 3% as the criterion for good stability. One part of Fuzi Lizhong Decoction solution was filtered through a 0.22 μm microporous membrane and injected at 0, 4, 8, 16, 24 and 48 h respectively for analysis. Each injection was 2 μL, and the RSD value of the Target-SIM extracted ion chromatogram peak area of ​​Fuzi Lizhong Decoction was calculated for each of the 6 injections. (5) Repeatability test: The repeatability test is based on RSD≤3% as the criterion for good repeatability. Six parallel solutions of Fuzi Lizhong Decoction were prepared and filtered through a 0.22 μm microporous membrane. 2 μL of each solution was injected into the membrane, and the RSD value of the mass fraction of each component in the six tested traditional Chinese medicine solutions was calculated.

[0019] (6) Recovery test: Dilute the Fuzi Lizhong Decoction solution by 2 times and take 40 μL to obtain test solution 1; Take 40 μL of the mixed reference solution diluted 100 times to obtain test solution 2; Test solution 1 and test solution 2 are mixed to obtain test solution 3; All test solutions were filtered through a 0.22 μm microporous membrane, and 2 μL of each solution was injected. The mass concentrations (C1, C2, and C3) of each compound in test solutions 1, 2, and 3 were calculated based on the corresponding standard curves. The recovery rate was calculated as (C3 - C1) / C2, and the RSD of the recovery rate was also calculated. A recovery rate within the range of 98% to 102% was considered acceptable.

[0020] (7) Limit of detection (LOD) and limit of quantification (LLOQ): The LOD and LLOQ of the 12 components were determined by a relatively intuitive method. Two samples with known component contents were added near the low concentration point of the standard curve for detection. A baseline near the analyte peak was selected as a reference, and the signal-to-noise ratio (S / N) of the chromatographic peaks of the 12 chemical components was calculated. The sample concentrations with S / N≥3 and S / N≥10 were used as LOD and LLOQ, respectively.

[0021] Experimental results: Results of methodological investigation (1) Systematic evaluation: Ion chromatograms of verbascoside, isoliquiritin, saflavin, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle were extracted using anhydrous ethanol blank reagent. Figure 1 Extracts of verbascoside, isoliquiritin, saflavin, gentianin, chrysanthemum flavonoids, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside ion chromatograms were obtained from a mixed standard solution. Figure 2 Comparing the two graphs, from top to bottom, the extracted ion chromatographic peaks of the following compounds are: verbascoside, isoglycyrrhizin, saflavin, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside. This shows that anhydrous ethanol has no significant interference with the determination of the contents of these 12 compounds. Detailed chromatographic-mass spectrometric data for these 12 compounds are shown in Table 1.

[0022] Table 1 Chromatographic-mass spectrometry data of 12 compounds (2) Linearity: The standard curve data of 12 compounds are shown in Table 2.

[0023] Table 2 Results of linear relationship investigation for 12 compounds (3) Precision test: The peak areas of the prepared reference standards verbascoside, isoglycyrrhizin, safflower flavonoid, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside were calculated, and their RSD results were 1.69%, 1.97%, 1.26%, 1.51%, 2.72%, 1.83%, 1.50%, 1.78%, 0.53%, 0.91%, 1.91%, and 0.59%, respectively. The results showed that the instrument precision was good.

[0024] (4) Stability test: The peak areas of the prepared Fuzi Lizhong Decoction sample, including isoflavone, isoglycyrrhizin, saflavin, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside, were calculated. The RSD results were 1.86%, 1.70%, 2.90%, 2.89%, 2.15%, 2.75%, 2.48%, 1.86%, 2.97%, 2.02%, 2.06%, and 2.91%, respectively. The results showed that the compounds had good stability within 48 hours.

[0025] (5) Repeatability test: The peak areas of the prepared Fuzi Lizhong Decoction sample, including isoflavone, isoliquiritin, ligustilide, senna flavonoid, gentianin, chrysanthemum flavonoid, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and lycopene, were calculated. The RSD results were 1.77%, 2.81%, 2.36%, 1.87%, 2.42%, 2.12%, 1.84%, 1.53%, 1.83%, 1.97%, 1.67%, and 1.97%, respectively. The results showed that the experiment had good repeatability.

[0026] (6) Spiking recovery test: The spiking recoveries of the prepared Fuzi Lizhong Decoction samples of isoflavone, isoliquiritin, ligustilide, sennain, gentiopicrin, chrysanthemumin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and lycopene were 99.53%, 98.85%, 99.35%, 100.21%, 99.58%, 99.37%, 98.97%, 99.15%, 99.37%, 100.51%, 99.43%, and 99.61%, respectively, with RSDs of 0.79%, 2.85%, 2.36%, 1.71%, 2.53%, 1.68%, 1.94%, 1.85%, 0.85%, 1.01%, 2.23%, and 1.33%, respectively. All were within the acceptable range, indicating that the recoveries of the 12 compounds were qualified.

[0027] (7) LOD and LLOQ: When S / N≥3, verbascoside, isoliquiritin, ligustilide, cinnamicin, The LODs of gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside were 0.002, 0.008, 0.016, 0.002, 0.052, 0.016, 0.003, 0.004, 0.002, 0.052, 0.160, and 0.052 ng / ml, respectively. When S / N ≥ 10, the LLOQs of verbascoside, isoliquiritigenin, ligustilide, cinnamyl flavonoid, gentiocarbazone, chrysanthemum flavonoid, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and lycopene were 0.004, 0.016, 0.080, 0.008, 0.160, 0.032, 0.016, 0.008, 0.008, 0.160, 0.320, and 0.160 ng / mL, respectively. Results of the determination of quality marker content in Fuzi Lizhong Decoction. The established method was used to determine the content of 12 quality markers in Fuzi Lizhong Decoction. The retention times and m / z values ​​of each component were consistent with the corresponding values ​​in Table 1, and they could be identified as 12 compounds. The content determination results showed that the average contents of verbascoside, isoglycyrrhizin, saflavin, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and lycopene were 0.042, 0.018, 0.002, 0.043, 0.026, 0.005, 0.152, 0.002, 0.158, 0.061, 0.008, and 0.004 μg / mL, respectively.

[0028] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any simple modifications, alterations, and equivalent changes made to the above embodiments based on the inventive essence shall still fall within the protection scope of the present invention.

Claims

1. A quality control method for a traditional Chinese medicine compound for gastric ulcers, characterized in that, The method is as follows: S1. Preparation of mixed reference solution: Weigh out the reference standards for verbascoside, isoglycyrrhizin, cheronitrile, styroside, gentianin, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohexadecanol, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside, respectively, and dilute to volume with anhydrous ethanol to obtain 12 reference solutions. Take equal volumes of each reference solution, mix them, and dilute to volume with anhydrous ethanol to obtain a mixed reference solution; S2. Preparation of the test Chinese herbal medicine solution: The traditional Chinese medicine for gastric ulcers was soaked in distilled water, extracted twice by reflux, and the two extracts were combined, filtered through gauze, concentrated in a rotary evaporator at 70°C, centrifuged, evaporated to dryness at 70°C, dissolved in anhydrous ethanol by ultrasonication, and brought to a final volume to obtain the test traditional Chinese medicine solution; the traditional Chinese medicine for gastric ulcers consisted of equal masses of Aconitum carmichaelii, Codonopsis pilosula, Zingiber officinale, Glycyrrhiza uralensis, and Atractylodes macrocephala. S3, Measurement: The mixed reference solution obtained in S1 and the test traditional Chinese medicine solution obtained in S2 were injected under the following liquid chromatography-tandem mass spectrometry conditions: S301, Liquid Chromatography Conditions: A 50 mm × 2.1 mm Hypersil Gold column with a particle size of 1.9 μm was used; the column temperature was 30 °C; the mobile phase was methanol + water; the gradient elution conditions were: 0–6 min, methanol volume ratio of mobile phase 25%–80%; 6 min–7 min, methanol volume ratio of mobile phase 80%–95%; 7 min–8 min, methanol volume ratio of mobile phase 95%–100%; 8 min–9 min, methanol volume ratio of mobile phase 100%; the flow rate was 0.3 mL / min. S302, Mass Spectrometry Conditions: Scanning mode: Full-MS / DD-MS2, simultaneous acquisition of positive and negative ions; positive ion scanning range 100 m / z~1500 m / z, negative ion scanning range 100 m / z~1500 m / z; resolution 17500; capillary temperature: 300℃; spray voltage: 4.0 kV and -3.5 kV; sheath gas volumetric flow rate 35 L / h; S-lens voltage 50 V; S4, Judgment: A blank solvent was set as a control. Under the conditions of liquid chromatography described in S301 and mass spectrometry described in S302, the presence of corresponding chemical components in the tested Chinese medicine solution was determined based on the chromatographic retention time and the precise molecular weight of the mass spectrometer. The mixed reference solution obtained in S1 was diluted into 5 mass concentration gradients. The mass concentration of each chemical component was plotted on the x-axis and the peak area on the y-axis. Standard working curves for 12 chemical components were plotted. The tested Chinese medicine solution obtained in S2 was quantified using the standard working curves. The response values ​​of the chemical components in the tested Chinese medicine solution were within the linear range of the instrument detection. The method for determining whether the corresponding chemical components exist in the tested traditional Chinese medicine solution is as follows: the chromatographic retention time and precise molecular weight information of the chemical components in the tested traditional Chinese medicine solution should be consistent with the information of the corresponding components in the mixed reference solution, with an allowable deviation of less than ±2.5%. The linear equation for verbascoside isoflavone is y = 1 × 10 12 x+1×10 7 r 2 =0.9951, with a linear range of 0.0032~0.16 μg / mL; The linear equation for isoliquiritigenin is y = 9 × 10 11 x + 7 × 10 6 r 2 =0.9965, with a linear range of 0.0032~0.16 μg / mL; The linear equation for saflavin is y = 8 × 10 10 x+236293, r 2 =0.9966, with a linear range of 0.0016~0.08 μg / mL; The linear equation for styracin is y = 5 × 10 11 x + 4 × 10 6 r 2 =0.9967, with a linear range of 0.0032~0.16 μg / mL; The linear equation for ternolactone is y = 1 × 10 11 x+867278, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone I is y = 6 × 10 11 x + 4 × 10 6 r 2 =0.9988, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone II is y = 9 × 10 11 x + 6 × 10 6 r 2 =0.9959, with a linear range of 0.0032~0.16 μg / mL; The linear equation for isohesperidin is y = 1 × 10 12 x+8×10 6 r 2 =0.9953, with a linear range of 0.0016~0.08 μg / mL; The linear equation for tyrosine is y = 4 × 10 10 x+846033, r 2 =0.9960, with a linear range of 0.0032~0.16 μg / mL; The linear equation for atractylodes lactone III is y = 1 × 10 10 x+36813, r 2 =0.9955, with a linear range of 0.0032~0.16 μg / mL; The linear equation for cryptochlorogenic acid is y = 1 × 10 11 x-173653, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The linear equation for lycopene is y = 8 × 10 10 x+52376, r 2 =0.9969, with a linear range of 0.0032~0.16 μg / mL; The contents of the chemical components contained in the traditional Chinese medicine were determined as follows: verbascoside, isoliquiritin, saflavin, styroside, chrysanthemum flavonoid, chrysanthemum lactone, atractylodes lactone I, atractylodes lactone II, isohesperidin, tyrosine, atractylodes lactone III, cryptochlorogenic acid, and honeysuckle glycoside.

2. The method for quality control of a traditional Chinese medicine compound for gastric ulcers according to claim 1, characterized in that, In S2, the first reflux extraction lasts for 30 minutes, and the second reflux extraction lasts for 20 minutes.

3. The method for quality control of a traditional Chinese medicine compound for gastric ulcers according to claim 1, characterized in that, The ratio of traditional Chinese medicine to distilled water used for gastric ulcers as described in S2 is 1g:10mL.

4. The method for quality control of a traditional Chinese medicine compound for gastric ulcers according to claim 1, characterized in that, The soaking time described in S2 is 30 minutes.

5. The method for quality control of a traditional Chinese medicine compound for gastric ulcers according to claim 1, characterized in that, The ultrasonic dissolution time described in S2 is 5 minutes.

6. The method for quality control of a traditional Chinese medicine compound for gastric ulcers according to claim 1, characterized in that, The centrifugation conditions in S2 are: 4℃, 10000rpm, 10min.

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