Patchouli qi-rectifying tablet and preparation process therefor, and quantitative and qualitative determination method for multiple components in patchouli qi-rectifying tablet

Abstract

A patchouli Qi-rectifying tablet, and a preparation method therefor and a qualitative and quantitative determination method therefor. The patchouli Qi-rectifying tablet comprises the following components in parts by mass: 0.5-1.5 parts of patchouli oil; 0.1-1 part of perilla leaf oil; 150-250 parts of common aucklandia root; 100-150 parts of rhizome of swordlike atractylodes; 10-100 parts of root of Ural licorice; 150-250 parts of Indian bread; 100-150 parts of dried tangerine peel; 100-150 parts of prepared tuber of pinellia; 100-150 parts of officinal magnolia bark; and 100-150 parts of fresh ginger. The qualitative and quantitative determination method for multiple components in the patchouli Qi-rectifying tablet comprises: performing qualitative determination of ten components, i.e., liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, atractylodin, perilla ketone, nobiletin, and tangeretin, in the patchouli Qi-rectifying tablet; and performing quantitative determination of seven components, i.e., liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodin, in the patchouli Qi-rectifying tablet. According to the method, the operation is simple, the detection time is short, the linear relationship is good, the repeatability is good, the precision is high, the accuracy is high, and the stability is good.

Description

A Zhengqi tablet and its preparation process and a method for quantitatively and qualitatively determining multiple components therein Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicine preparation and traditional Chinese medicine component detection, and relates to a Zhengqi tablet and a preparation process thereof and a quantitative and qualitative determination method of multiple components therein. Background Art

[0002] Zhengqi Tablets are traditional Chinese patent medicines, mainly used to treat colds, headaches, chest tightness, vomiting, diarrhea, abdominal distension, etc. It can relieve heat and dampness, and is mostly used for fever, chest tightness, abdominal distension, vomiting and diarrhea caused by exogenous heat and dampness. It can also soothe the stomach and stop vomiting, and is mostly used for nausea and vomiting caused by excessive dampness and turbidity. At the same time, it can aromaticize turbidity, and is commonly used for symptoms such as loss of appetite, thick and greasy tongue coating, and diarrhea caused by spleen dampness and stomach turbidity. It belongs to the Huoxiang Zhengqi series of products, but there are significant differences in the prescription, prescription amount and process between Zhengqi Tablets and Huoxiang Zhengqi Tablets (pills, drops). The material basis of the two is quite different, and they belong to different Chinese patent medicines. Therefore, for the composition, preparation and quantitative and qualitative detection of the ingredients contained in Zhengqi Tablets, it is impossible to refer to Huoxiang Zhengqi Tablets.

[0003] Currently, various research projects are underway on Zhengqi tablets. Traditional Chinese medicine fingerprints, characterized by holistic, macroscopic, and fuzzy analysis, can achieve holistic quality control by describing the overall characteristics of a traditional Chinese medicine and employing appropriate fuzzy processing. Therefore, they have become an effective tool for quality control of traditional Chinese medicine. Chromatographic fingerprint analysis can visualize the overall characteristics of multiple chemical components within a traditional Chinese medicine, thereby revealing quality issues that are difficult to detect through conventional testing. However, traditional Chinese medicine fingerprints are not capable of quantitatively and qualitatively determining the numerous components within a traditional Chinese medicine. Chinese Patent 2018109246518 established a high-performance liquid chromatography fingerprint for Zhengqi tablets, but did not quantitatively and qualitatively determine the components within the tablets. Chinese Patent 2020113871985 established a gas chromatography fingerprint for Zhengqi tablets, but only identified three indicator components, but also failed to quantitatively and qualitatively determine the components within the tablets. Furthermore, Chinese Patent 2022110331062 only quantitatively determined four components in the Zhengqi tablet extract, an intermediate for Zhengqi tablets. It can be seen that the research on Zhengqi Tablets is not comprehensive, and there is a lack of rapid quantitative and qualitative determination of the many components in Zhengqi Tablets.

[0004] Summary of the Invention

[0005] In view of the shortcomings of the prior art mentioned above, the purpose of the present invention is to provide a Zhengqi tablet and its preparation process and a method for quantitative and qualitative determination of multiple components therein, which can provide Zhengqi tablets with stable quality and low unqualified rate, and through a reliable preparation method and quantitative and qualitative determination of 10 components in Zhengqi tablets, solve the lack of the prior art. By quantitative and qualitative determination of multiple components in Zhengqi tablets, the quality of Zhengqi tablets can be objectively, comprehensively and accurately evaluated, which is of great significance for controlling the quality of Zhengqi tablets and ensuring clinical efficacy.

[0006] To achieve the above-mentioned and other related objects, the present invention provides a Zhengqi tablet in a first aspect, comprising the following components, measured by mass: 0.5-1.5 parts of patchouli oil; specifically, 0.5-0.8 parts, 0.8-1.2 parts, or 1.2-1.5 parts; 0.1-1 parts of perilla leaf oil; specifically, 0.1-0.4 parts, 0.4-0.8 parts, or 0.8-1 parts; 150-250 parts of costus root; specifically, 150-180 parts, 180-220 parts, or 220-250 parts; 100-150 parts of atractylodes; specifically, 100-130 parts, 130-140 parts, or 140-150 parts; 10-100 parts of licorice; specifically, 10-60 parts, 60-70 parts, or 70-100 parts; 150-250 parts of Poria cocos; specifically 150-180 parts, 180-220 parts, 220-250 parts; 100-150 parts of dried tangerine peel; specifically 100-130 parts, 130-140 parts, 140-150 parts; 100-150 parts of processed Pinellia ternata; specifically 100-130 parts, 130-140 parts, 140-150 parts; 100-150 parts of Zingiber officinale; specifically 100-130 parts, 130-140 parts, 140-150 parts; 100-150 parts of ginger; specifically 100-130 parts, 130-140 parts, 140-150 parts.

[0007] Preferably, the Zhengqi tablets comprise the following components in parts by mass: 0.8-1.2 parts of patchouli oil; 0.4-0.8 parts of perilla leaf oil; 180-220 parts of costus root; 130-140 parts of atractylodes; 60-70 parts of liquorice; 180-220 parts of poria; 130-140 parts of tangerine peel; 130-140 parts of processed pinellia; 130-140 parts of ginger magnolia bark; and 130-140 parts of ginger.

[0008] Preferably, the Zhengqi tablets comprise the following components in parts by mass: 1.0 part of patchouli oil; 0.6 part of perilla leaf oil; 200 parts of costus root; 133 parts of atractylodes; 67 parts of liquorice; 200 parts of poria; 133 parts of tangerine peel; 133 parts of processed pinellia; 133 parts of ginger magnolia bark; and 133 parts of ginger.

[0009] Preferably, the patchouli oil and perilla oil should be precisely weighed.

[0010] Preferably, the costus root (Aucklandiae Radix), atractylodes (Atractylodis Rhizoma), liquorice (Glycyrrhizae Radix et Rhizoma), poria (Poria), tangerine peel (Citri Reticulatae Pericarpium), pinellia (Pinelliae Rhizoma), magnolia bark (Magnoliae officinalis Cortex), and ginger (Zingiberis Rhizoma Recens) are accurately weighed and then ground into powder. The pinellia is processed pinellia, the magnolia bark is ginger magnolia bark, and the ginger is fresh ginger.

[0011] The patchouli oil is an extract from the genus Echinops of the Lamiaceae family. The perilla leaf oil is an extract from the perilla leaf of the annual upright herb of the dicotyledonous family of the Lamiaceae family. The costus root is the dried root of the costus root of the Asteraceae family. Atractylodes lancea is the dried rhizome of Atractylodes macrocephala or Atractylodes macrocephala of the Asteraceae family. Licorice is the dried root and rhizome of Glycyrrhiza uralensis, Glycyrrhiza glabra or Glycyrrhiza glabra of the Leguminosae family. Poria is the dried sclerotium of the fungus Poria of the Polyporaceae family. Tangerine peel is the dried mature peel of the citrus plant and its cultivated varieties of the Rutaceae family. Pinellia is the dried tuber of the Pinellia plant of the Araceae family. Magnolia officinalis is the dried bark, root bark and branch bark of Magnolia officinalis or Magnolia officinalis of the Magnoliaceae family. Ginger is the fresh rhizome of the perennial herb Zingiber officinale of the Zingiberaceae family.

[0012] A second aspect of the present invention provides a preparation process of a positive energy tablet, comprising the following steps:

[0013] 1) mixing the first part of costus root, atractylodes lancea, and liquorice according to the proportion, grinding them into powder, and sieving to obtain a powder;

[0014] 2) boiling the second portion of Poria cocos, dried tangerine peel, processed Pinellia ternata, Magnolia officinalis bark, ginger, and licorice root in water according to the proportions, filtering and concentrating the decoction to obtain a paste;

[0015] 3) The paste and powder are mixed and granulated, patchouli oil and perilla leaf oil are added according to the proportion, and the mixture is pressed into tablets.

[0016] Preferably, in step 1) or 2), the mass ratio of the first part of licorice to the second part of licorice is 55-65:35-45, specifically 55-60:40-45, 60-65:35-40, preferably 60:40.

[0017] Preferably, in step 1), sucrose is also added during the mixing.

[0018] Preferably, the mass ratio of the sucrose to costus root is 25-30:150-250, specifically 25-30:150-180, 25-30:180-220, 25-30:220-250, preferably 27:180-220, more preferably 27:200.

[0019] Preferably, in step 1), the mesh size of the sieve is 80-120 meshes, preferably 100 meshes.

[0020] Preferably, in step 2), the decocting step is performed until boiling.

[0021] Preferably, in step 2), the decocting is performed at least 2 times, preferably 2 times.

[0022] Preferably, when the decoction is performed twice, the first decoction time is 2-4 hours, preferably 3 hours; the second decoction time is 1-3 hours, preferably 2 hours.

[0023] Preferably, when the decoction is performed twice, the amount of water added in the first decoction is 7.5-8.5 times, preferably 8 times; the amount of water added in the second decoction is 5.5-6.5 times, preferably 6 times.

[0024] The decoction is obtained by combining at least 2 decoctions.

[0025] Preferably, in step 2), the filtration is performed using a blue filter. The blue filter is a commonly used blue filter.

[0026] Preferably, in step 2), the concentration temperature is 50-70°C.

[0027] Preferably, in step 2), the concentration is performed to a relative density of 1.03-1.05, thereby obtaining a dense paste.

[0028] Preferably, in step 3), when the paste and the powder are mixed, a suitable amount of water is added to the paste. The suitable amount of water added refers to adding water until the paste becomes flowable.

[0029] Preferably, in step 3), the granulation is a conventional granulation process. Specifically, the granulation is carried out by placing the powder as the base material into a fluidized bed granulator according to the division of the granulation ingredients, and spraying the material paste into the granulator for granulation.

[0030] Preferably, in step 3), a lubricant is also added when the patchouli oil and perilla leaf oil are added.

[0031] Preferably, the lubricant is talc.

[0032] Preferably, the lubricant is added in an amount of 1.5-2.5% by weight of the particles, preferably 2%.

[0033] Preferably, in step 3), the tableting is performed using a conventional tableting process for traditional Chinese medicine tablets.

[0034] The third aspect of the present invention provides a positive energy tablet prepared by the above process.

[0035] The fourth aspect of the present invention provides a method for quantitatively and qualitatively determining multiple components in Zhengqi tablets, comprising: dissolving Zhengqi tablets in methanol, performing ultrasonic extraction, cooling, filtering the supernatant, and detecting the obtained test solution using ultra-performance liquid chromatography (UPLC). The 10 components in the test solution are qualitatively determined: liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin; and the contents of the 7 components in the test solution are quantitatively determined: liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, and atractylodesin.

[0036] Preferably, the CAS number of the liquiritin is 551-15-5, the CAS number of hesperidin is 520-26-3, the CAS number of honokiol is 35354-74-6, the CAS number of costunolide is 553-21-9, the CAS number of dehydrocostus lactone is 74299-48-2, the CAS number of magnolol is 528-43-8, the CAS number of atractylodesin is 55290-63-6, the CAS number of perillone is 142546-15-4, the CAS number of nobiletin is 478-01-3, and the CAS number of tangeretin is 481-53-8.

[0037] Preferably, the ratio of the mass g of the added Zhengqi tablets to the volume mL of the added methanol is 0.3:15-25, preferably 0.3:20.

[0038] Preferably, the ultrasonic extraction time is 30-60 minutes, preferably 40-50 minutes, more preferably 45 minutes.

[0039] Preferably, the power of the ultrasonic extraction is 200-350W, preferably 250W; the frequency of the ultrasonic extraction is 40-60kHz, preferably 40kHz.

[0040] Preferably, the cooling is performed to room temperature, which is 20-30°C.

[0041] Preferably, the filtration is to take the supernatant and filter it through a membrane.

[0042] Preferably, the filter membrane is a 0.22 μm filter membrane.

[0043] Preferably, the detection using ultra-performance liquid chromatography (UPLC) comprises the following steps:

[0044] A1) Preparation of reference solution: Dissolve reference substances of liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin in methanol and dilute to volume to prepare a reference solution;

[0045] A2) Sample Assay: The test solution and the reference solution from step A1) were assayed by ultra performance liquid chromatography (UPLC) by comparing retention times for qualitative analysis and by external standard analysis for quantitative analysis. Ten components in the test solution were qualitatively determined: liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. Seven components in the test solution were quantitatively determined: liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, and atractylodesin.

[0046] Ultra Performance Liquid Chromatography (UPLC) differs from traditional High Performance Liquid Chromatography (HPLC) by incorporating novel technologies such as small particle size, very low system volume, and rapid detection methods, increasing analytical throughput, sensitivity, and chromatographic peak capacity. Compared to HPLC, which suffers from lengthy detection times, complex chromatographic peaks, and reduced resolution, UPLC's detection speed, sensitivity, and resolution are unmatched by HPLC. UPLC's speed, sensitivity, and resolution are 9 times, 3 times, and 1.7 times, respectively, of HPLC. This shortens analysis time, reduces solvent usage, and lowers analytical costs.

[0047] Preferably, in step A1), the reference solution is shaken and filtered to obtain a filtrate.

[0048] Preferably, in step A1), the reference solution is prepared by serial dilution. Specifically, a stock solution is first prepared and then diluted with methanol to form the reference solution. The stock solution is stored in a refrigerator at 4°C away from light.

[0049] Preferably, in step A1), the content of liquiritin in the reference solution is in the range of 4.52-45.22 μg / ml, preferably 10 μg / ml; the content of hesperidin is in the range of 9.50-237.61 μg / ml, preferably 50 μg / ml; the content of honokiol is in the range of 1.98-49.50 μg / ml, preferably 10 μg / ml; the content of costunolide is in the range of 10.44-261.14 μg / ml, preferably 50 μg / ml; the content of dehydrocostus lactone is in the range of 21.49-5 31.30μg / ml, preferably 100μg / ml; the content range of magnolol is 1.79-44.86μg / ml, preferably 10μg / ml; the content range of atractylodesin is 1.92-47.96μg / ml, preferably 10μg / ml; the content range of perilla ketone is 15-25μg / ml, preferably 20μg / ml; the content range of nobiletin is 40-60μg / ml, preferably 50μg / ml; the content range of tangeretin is 15-25μg / ml, preferably 20μg / ml.

[0050] Preferably, in step A2), in the ultra performance liquid chromatography (UPLC), the detector is a diode array detector (DAD).

[0051] Preferably, in step A2), the chromatographic column used in the ultra-high performance liquid chromatography method is a T3 chromatographic column.

[0052] More preferably, the chromatographic column used in the ultra-high performance liquid chromatography method is a Waters Acquity UPLC HSS T3 chromatographic column (column length: 100 mm, inner diameter: 2.1 mm, filler particle size: 1.8 μm).

[0053] Preferably, in step A2), the detection wavelength in the ultra-high performance liquid chromatography method is 224-226 nm. More preferably, the detection wavelength is 225 nm.

[0054] Preferably, in step A2), the column temperature in the ultra-high performance liquid chromatography method is 30-45°C, specifically 30-35°C, 35-45°C, 32-38°C, preferably 35°C.

[0055] Preferably, in step A2), the flow rate of the ultra-high performance liquid chromatography is 0.1 to 0.3 mL / min. More preferably, the flow rate of the ultra-high performance liquid chromatography is 0.2 mL / min.

[0056] Preferably, in step A2), the injection volume in the ultra-high performance liquid chromatography method is 0.5 to 5 μL. More preferably, the injection volume in the ultra-high performance liquid chromatography method is 1 μL.

[0057] Preferably, in step A2), in the ultra-high performance liquid chromatography method, the mobile phase is acetonitrile-0.05-0.15% formic acid aqueous solution, wherein phase A is acetonitrile and phase B is 0.05-0.15% formic acid aqueous solution; the analysis time is 19 minutes; and gradient elution is used.

[0058] More preferably, in the ultra-high performance liquid chromatography method, the mobile phase is acetonitrile-0.10% formic acid aqueous solution, wherein phase A is acetonitrile and phase B is 0.10% formic acid aqueous solution; the analysis time is 19 minutes; and gradient elution is used.

[0059] The above-mentioned 0.05-0.15% formic acid aqueous solution is a formic acid aqueous solution with a volume percentage of 0.05-0.15%. The above-mentioned 0.10% formic acid aqueous solution is a formic acid aqueous solution with a volume percentage of 0.10%.

[0060] More preferably, the specific procedure of the gradient elution is shown in Table 1, which is:

[0061] 0-4 min, the volume ratio of phase A:phase B was 20:80-35:65;

[0062] 4-5 min, the volume ratio of phase A:phase B is 35:65-40:60;

[0063] 5-6 min, the volume ratio of phase A:phase B is 40:60-55:45;

[0064] 6-15 min, the volume ratio of phase A:phase B is 55:45-60:40;

[0065] 15-16 min, the volume ratio of phase A:phase B is 60:40-90:10;

[0066] 16-19 min, the volume ratio of phase A:phase B is 90:10-90:10.

[0067] The analysis time of this determination method is only 19 minutes, and it can quickly determine the 10 components in Zhengqi tablets in a short time. It not only saves reagents but also greatly reduces the daily QC testing work.

[0068] Table 1

[0069] Preferably, in step A2), the external standard method comprises the following steps:

[0070] A) preparing a series of reference solution solutions of varying concentrations according to step A1), and performing UPLC analysis on each solution to obtain linear relationships between the chromatographic peak areas of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin and the corresponding contents of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin, plotting corresponding standard working curves, and calculating regression equations for the standard working curves of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin, respectively;

[0071] B) The test solution was subjected to UPLC detection, and the obtained chromatographic peak areas of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin were substituted into the regression equation of the standard working curve of the corresponding liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin in step A) to calculate the content of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin in the test solution.

[0072] More preferably, in the standard working curve, the chromatographic peak areas of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin are used as the ordinate (Y-axis), and the corresponding contents (i.e., concentrations) of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin are used as the abscissa (X-axis).

[0073] In the ultra-performance liquid chromatography (UPLC) detection, the above-mentioned perillone, nobiletin and tangeretin are not suitable as quantitative indicators because the peak areas of perillone and tangeretin are too small and the content is too low, which does not meet the general content requirements (≥0.02%). At the same time, according to the provisions of the "Chinese Pharmacopoeia", when quantifying, the separation between the chromatographic peak of the substance to be tested and the adjacent chromatographic peak should be greater than 1.5. Perillone, nobiletin and tangeretin do not meet this requirement, so they can only be qualitative.

[0074] As described above, the present invention provides a Zhengqi tablet, a preparation process thereof, and a method for quantitatively and qualitatively determining multiple components therein, which determine the components of the Zhengqi tablet and its preparation, and adopts optimized pretreatment conditions and UPLC instrument detection method, which can quickly qualitatively determine the 10 components in the Zhengqi tablet in a very short time, such as 19 minutes, and quickly quantify 7 of the components (liquiritin, hesperidin, honokiol, magnolol, costunolide, dehydrocostus lactone and atractylodesin). This method is simple to operate, highly reproducible, and easy to control. It also features simple pretreatment, resolving issues previously encountered with hesperidin, such as complex pretreatment and poor parallelism. It can simultaneously detect multiple components and significantly shortens detection time. This method facilitates front-end control of medicinal materials. Liquiritin is the primary component of licorice, hesperidin is the primary component of dried tangerine peel, honokiol and magnolol are the primary components of ginger magnolia bark, costunolide and dehydrocostus lactone are the primary components of costus root, and atractylodesin is the primary component of atractylodes. Therefore, while controlling the quality of the compound, it is possible to simultaneously control the five medicinal materials—licorice, dried tangerine peel, ginger magnolia bark, costus root, and atractylodes—to ensure stable production and clinical efficacy. The standard curves for the seven components determined by this method exhibit good linearity within their respective ranges, with good reproducibility, precision, accuracy, and stability. This method can be used to accumulate data from multiple batches of samples and establish reasonable content limits to ensure stable production and clinical efficacy.

[0075] Compared with the prior art, the present invention has obvious detection advantages. For example, Chinese Patent 2018109246518 only provides the HPLC fingerprint of Zhengqi Tablets obtained by the gradient elution program with an analysis time of 115 minutes, and does not perform quantitative and qualitative analysis on any components in Zhengqi Tablets. For another example, Chinese Patent 2020113871985 only provides the GC fingerprint of Zhengqi Tablets obtained by the heating program, and does not perform quantitative and qualitative analysis on any components in Zhengqi Tablets. For another example, although Chinese Patent 2022110331062 performed quantitative and qualitative analysis of components, its analysis object was Zhengqi Tablets extract, and only quantitative and qualitative analysis of 4 components in the Zhengqi Tablets extract obtained by the gradient elution program with an analysis time of 34 minutes was performed.

[0076] Compared with Chinese Patent 2018109246518, the detection instrument UPLC used in the present invention is superior to the detection instrument HPLC used therein; compared with Chinese Patent 2020113871985, the detection instrument UPLC used in the present invention is completely different from the detection instrument GC used therein; compared with Chinese Patent 2022110331062, the analysis object of the present invention is Zhengqi Tablets. It is different from the Zhengqi Tablets extract which is the intermediate of Zhengqi Tablets. It is particularly worth noting that the present invention only provides a gradient elution program with an analysis time of 19 minutes, and its detection time is much shorter than the above-mentioned prior art. It can simultaneously qualitatively analyze 10 components and quantitatively analyze 7 components, which greatly saves the amount of solvent and reduces costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0077] Figure 1 shows a chromatogram for the specificity investigation of the ingredients in the present invention, wherein S1 is a Zhengqi Tablet sample lacking costus root and atractylodes lancea, S2 is a Zhengqi Tablet sample lacking atractylodes lancea, S3 is a Zhengqi Tablet sample lacking costus root, S4 is a Zhengqi Tablet sample lacking ginger and magnolia bark, S5 is a Zhengqi Tablet sample lacking tangerine peel, S6 is a Zhengqi Tablet sample lacking liquorice, S7 is a Zhengqi Tablet sample, and S8 is a reference substance; 1 is liquiritin, 2 is hesperidin, 3 is magnolol, 4 is costunolide, 5 is dehydrocostus lactone, 6 is magnolol, and 7 is atractylodesin.

[0078] Figure 2 shows the UPLC chromatograms of the test sample and the reference sample in the present invention, wherein S1 is the UPLC chromatogram of the test sample, and S2 is the UPLC chromatogram of the reference sample; 1 is liquiritin, 2 is hesperidin, 3 is perilla ketone, 4 is nobiletin, 5 is tangeretin, 6 is honokiol, 7 is costunolide, 8 is dehydrocostus lactone, 9 is magnolol, and 10 is atractylodesin. DETAILED DESCRIPTION

[0079] The present invention is further described below with reference to specific examples. It should be understood that these examples are only used to illustrate the present invention and are not used to limit the scope of protection of the present invention.

[0080] The following describes the embodiments of the present invention through specific examples. Those skilled in the art will readily understand the other advantages and benefits of the present invention from the disclosure herein. The present invention may also be implemented or applied through various other specific embodiments, and the details in this specification may be modified or altered based on different viewpoints and applications without departing from the spirit of the present invention.

[0081] The reagents and instruments used in the following examples are as follows:

[0082] 1. Reagents

[0083] Ten batches of Zhengqi tablets (batch numbers 200401, 200402, 210101, 210102, 21010601, 21010701, 210201, 210204, 210901, and 210902, prepared by Shanghai Hutchison Pharmaceuticals Co., Ltd.); negative samples (Gancao Zhengqi tablets missing, Chenpi Zhengqi tablets missing, Houpo Zhengqi tablets missing, and Atractylodes Zhengqi tablets missing) were all provided by Shanghai Hutchison Pharmaceuticals Co., Ltd.

[0084] Reference substances: liquiritin (batch number 111610-201908, mass fraction 95%), hesperidin (batch number 110721-201818, mass fraction 96.2%), honokiol (batch number 110730-201915, mass fraction 99.8%), magnolol (batch number 110729-201513, mass fraction 98.8%), costunolide (batch number 111524-201911, mass fraction 99.9%), dehydrocostus lactone (batch number 111525-201912, mass fraction 99.5%), atractylodesin (batch number 111924-201806, mass fraction 99.5%). All of the above reference substances were purchased from the China Food and Drug Inspection Institute. Perillone (batch number 1681-025A1, mass fraction 98.7%) was purchased from TLC Pharmaceutical Standards Ltd., Canada. Nobiletin (batch number 6082, mass fraction 98.7%) and tangeretin (batch number 6083, mass fraction 99.5%) were purchased from Shanghai Shidande Standard Technology Service Co., Ltd.

[0085] Reagents: anhydrous methanol (analytical grade AR, Sinopharm Chemical Reagent Co., Ltd.); acetonitrile (chromatographic grade, TEDIA, USA); formic acid (chromatographic grade, TEDIA, USA); ultrapure water was prepared using a Milli-Q ultrapure water treatment system.

[0086] 2. Instruments

[0087] A Waters Acquity UPLC H-Class ultra-high performance liquid chromatograph (equipped with an Empower 3 chromatography workstation, a quaternary ultrahigh pressure solvent manager, an automatic sample manager, a column oven, and a PDAeλ detector, all from Waters, USA) was used; an SB-5200DTD ultrasonic cleaner was used (Ningbo Xinzhi Biotechnology Co., Ltd.); AL204 and XS205 analytical electronic balances were used (METTLER TOLEDO Instruments Shanghai Co., Ltd.); and a Milli-Q Advantage A10 ultrapure water system was used (Merck Millipore, Germany).

[0088] Example 1

[0089] Take 200g of costus root, 133g of atractylodes, and 40.2g of the first portion of licorice, add 27g of sucrose, and grind into a fine powder. Pass through a 100-mesh sieve to obtain powder 1#. Take the second portion of 200g of poria, 133g of dried tangerine peel, 133g of processed pinellia, 133g of ginger magnolia bark, 133g of ginger, and 26.8g of licorice, and decoct twice with water. The first time, add 8 times the amount of water and boil for 3 hours. The second time, add 6 times the amount of water and boil for 2 hours. The decoctions are combined, filtered through a blue filter, and concentrated at 60°C to a relative density of 1.04 to obtain paste 1#. The paste 1# and the powder 1# were mixed and granulated. When the paste and the powder were mixed, an appropriate amount of water was added to the paste until the paste became flowable. Then 1.0 g of patchouli oil, 0.6 g of perilla leaf oil and 2% of the weight of the particles of talcum powder were added, and the mixture was pressed into 1000 tablets to obtain Zhengqi Tablet Sample 1#.

[0090] Example 2

[0091] Take 190g of costus root, 130g of atractylodes, and the first portion of 36g of licorice, add 27g of sucrose, and grind them into a fine powder. Pass through a 110-mesh sieve to obtain powder 2#. Take the second portion of 190g of poria, 130g of dried tangerine peel, 130g of processed pinellia, 130g of ginger magnolia bark, 130g of ginger, and 24g of licorice, and decoct them twice in water. The first time, add 8.5 times the amount of water and boil for 3.5 hours. The second time, add 6.5 times the amount of water and boil for 2.5 hours. Combine the decoctions, filter through a blue filter, and concentrate at 65°C to a relative density of 1.05 to obtain paste 2#. The paste 2# and the powder 2# were mixed and granulated. When the paste and the powder were mixed, an appropriate amount of water was added to the paste until the paste was flowable. Then 0.9g of patchouli oil, 0.5g of perilla leaf oil and 2.5% of the weight of the particles of talcum powder were added, and pressed into 1000 tablets to obtain Zhengqi Tablet Sample 2#.

[0092] Example 3

[0093] 1. Preparation of test solution

[0094] Take 0.3 g of the Zhengqi tablet sample 1# prepared in Example 1, accurately weigh it, place it in a 50 mL centrifuge tube, accurately add 20 mL of methanol, ultrasonically extract (250w, 40kHz) for 45 minutes, let it cool to room temperature, take the supernatant and pass it through a 0.22 μm filter membrane, take the filtrate to obtain the test solution 1#.

[0095] 2. Preparation of reference solution

[0096] Accurately weigh the reference substances of liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. Dissolve them in methanol in a 100 mL volumetric flask to the desired volume to prepare the reference substance stock solution. Store the reference substance stock solution in a refrigerator at 4°C, protected from light.

[0097] The reference substance stock solution was then diluted with methanol and fixed to volume to prepare a series of reference substance solutions of different concentrations. In the series of reference substance solutions of different concentrations, the content of liquiritin ranged from 4.52 to 45.22 μg / ml; the content of hesperidin ranged from 9.50 to 237.61 μg / ml; the content of honokiol ranged from 1.98 to 49.50 μg / ml; the content of costunolide ranged from 10.44 to 261.14 μg / ml; the content of dehydrocostus lactone ranged from 21.49 to 531.30 μg / ml; the content of magnolol ranged from 1.79 to 44.86 μg / ml; the content of atractylodesin ranged from 1.92 to 47.96 μg / ml; the content of perillone ranged from 20 μg / ml; the content of nobiletin ranged from 50 μg / ml; and the content of tangeretin ranged from 20 μg / ml. The reference solution should also be shaken and filtered to obtain the filtrate.

[0098] 3. Determination

[0099] Ultra performance liquid chromatography (UPLC) was used to detect the test solution 1# and a series of reference solutions with different concentrations. The retention times were compared for qualitative analysis, and the external standard method was used for quantitative analysis. That is, the retention times were compared to determine the 10 components in the test solution: liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin and tangeretin. Then a series of reference solutions with different concentrations were subjected to UPLC detection to obtain the linear relationship between the chromatographic peak areas of liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol and atractylodesin and the corresponding contents of liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol and atractylodesin. The corresponding standard working curves were drawn and the regression equations of the standard working curves of liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol and atractylodesin were calculated respectively. The test solution 1# was then subjected to UPLC detection, and the chromatographic peak areas of the obtained liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, and atractylodesin were substituted into the regression equation of the standard working curve of the corresponding liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, and atractylodesin to calculate the contents of liquiritin, hesperidin, honokiol, costunol, dehydrocostus lactone, magnolol, and atractylodesin in the test solution.

[0100] Among them, the high performance liquid chromatography method includes the following detection conditions:

[0101] The detector was a diode array detector (DAD); the chromatographic column was a Waters Acquity UPLC HSS T3 column (column length: 100 mm, inner diameter: 2.1 mm, filler particle size: 1.8 μm); the detection wavelength was 225 nm; the column temperature was 35°C; the flow rate was 0.2 mL / min; the injection volume was 1 μl; the mobile phase was acetonitrile-0.10% formic acid aqueous solution, wherein phase A was acetonitrile and phase B was 0.10% formic acid aqueous solution; the analysis time was 19 min; and gradient elution was used.

[0102] The specific procedure of gradient elution is:

[0103] 0-4 min, the volume ratio of phase A:phase B was 20:80-35:65;

[0104] 4-5 min, the volume ratio of phase A:phase B is 35:65-40:60;

[0105] 5-6 min, the volume ratio of phase A:phase B is 40:60-55:45;

[0106] 6-15 min, the volume ratio of phase A:phase B is 55:45-60:40;

[0107] 15-16 min, the volume ratio of phase A:phase B is 60:40-90:10;

[0108] 16-19 min, the volume ratio of phase A:phase B is 90:10-90:10.

[0109] Example 4

[0110] 1. Preparation of test solution

[0111] Take 0.3 g of the Zhengqi tablet sample 1# prepared in Example 1, accurately weigh it, place it in a 50 mL centrifuge tube, accurately add 15 mL of methanol, ultrasonically extract (240w, 35kHz) for 40 minutes, let it cool to room temperature, take the supernatant and pass it through a 0.22 μm filter membrane, take the filtrate to obtain the test solution 2#.

[0112] 2. Preparation of reference solution

[0113] Accurately weigh the reference substances of liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. Dissolve them in methanol and bring to volume in a 100 mL volumetric flask to prepare a reference substance stock solution. Store the reference substance stock solution in a refrigerator at 4°C, protected from light. Dilute the reference substance stock solution with methanol and bring to volume to prepare a series of reference substance solutions of varying concentrations.

[0114] In a series of reference solutions with different concentrations, the concentration ranges of liquiritin, hesperidin, honokiol, costus lactone, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin and tangeretin were the same as those in step 2 of Example 3.

[0115] 3. Determination

[0116] Ultra-high performance liquid chromatography (UPLC) was used to detect the test solution 2# and a series of reference solutions of different concentrations. The retention times were compared for qualitative analysis. The external standard method was used for quantitative analysis. The retention times were compared to determine the 10 components in the test solution: liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. The concentrations of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin in the test solution 2# were determined. The specific quantitative process was the same as step 3 in Example 3.

[0117] Among them, the high performance liquid chromatography method includes the following detection conditions:

[0118] The detector was a diode array detector (DAD); the chromatographic column was a Waters Acquity UPLC HSS T3 column (column length: 100 mm, inner diameter: 2.1 mm, filler particle size: 1.8 μm); the detection wavelength was 224 nm; the column temperature was 30°C; the flow rate was 0.1 mL / min; the injection volume was 0.5 μL; the mobile phase was acetonitrile-0.15% formic acid aqueous solution, wherein phase A was acetonitrile and phase B was 0.15% formic acid aqueous solution; the analysis time was 34 min; and gradient elution was used.

[0119] The specific procedure of gradient elution is the same as step 3 in Example 3.

[0120] Example 5

[0121] 1. Preparation of test solution

[0122] Take 0.3 g of the Zhengqi tablet sample 1# prepared in Example 1, accurately weigh it, place it in a 50 mL centrifuge tube, accurately add 25 mL of methanol, ultrasonically extract (260w, 45kHz) for 50 minutes, let it cool to room temperature, take the supernatant and pass it through a 0.22 μm filter membrane, take the filtrate to obtain the test solution 3#.

[0123] 2. Preparation of reference solution

[0124] Accurately weigh the reference substances of liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. Dissolve them in methanol and bring to volume in a 100 mL volumetric flask to prepare a reference substance stock solution. Store the reference substance stock solution in a refrigerator at 4°C, protected from light. Dilute the reference substance stock solution with methanol and bring to volume to prepare a series of reference substance solutions of varying concentrations.

[0125] In a series of reference solutions with different concentrations, the concentration ranges of liquiritin, hesperidin, honokiol, costus lactone, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin and tangeretin were the same as those in step 2 of Example 3.

[0126] 3. Determination

[0127] Ultra-high performance liquid chromatography (UPLC) was used to detect the test solution 3# and a series of reference solutions of different concentrations. The retention times were compared for qualitative analysis. The external standard method was used for quantitative analysis. The retention times were compared to determine the concentrations of 10 components in the test solution: liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, atractylodesin, perillone, nobiletin, and tangeretin. The concentrations of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin in the test solution 3# were determined. The specific quantitative process was the same as step 3 in Example 3.

[0128] Among them, the high performance liquid chromatography method includes the following detection conditions:

[0129] The detector was a diode array detector (DAD); the chromatographic column was a Waters Acquity UPLC HSS T3 column (column length: 100 mm, inner diameter: 2.1 mm, filler particle size: 1.8 μm); the detection wavelength was 226 nm; the column temperature was 45°C; the flow rate was 0.3 mL / min; the injection volume was 2 μL; the mobile phase was acetonitrile-0.05% formic acid aqueous solution, wherein phase A was acetonitrile and phase B was 0.05% formic acid aqueous solution; the analysis time was 19 min; and gradient elution was used.

[0130] The specific procedure of gradient elution is the same as step 3 in Example 3.

[0131] Example 6

[0132] Take Zhengqi Tablet sample 1# prepared in Example 1 and prepare a test solution according to step 1 in Example 3. Simultaneously, take a negative sample of Zhengqi Tablet lacking flavor, removing licorice, dried tangerine peel, magnolia bark, costus root, and atractylodes, and prepare a negative test solution according to step 1 in Example 3. In addition, prepare a reference solution according to step 2 in Example 3.

[0133] The above-mentioned test solution, negative test solution, and reference solution were measured according to step 3 of Example 3, and the retention time was compared for qualitative analysis. The specific test results are shown in Figure 1. As shown in Figure 1, there is no negative interference in the 7 chromatographic peaks, and the method has good specificity. Among them, peak 1 is liquiritin, which comes from licorice medicinal material; peak 2 is hesperidin, which comes from tangerine peel medicinal material; peak 3 is magnolol, and peak 6 is magnolol, both of which come from ginger magnolia bark medicinal material; peak 4 is costunolide, and peak 5 is dehydrocostus lactone, both of which come from costus root medicinal material; peak 7 is atractylodesin, which comes from atractylodes and costus root medicinal material.

[0134] Example 7

[0135] The quantitative and qualitative determination method of multiple components in the Zhengqi tablet sample of the present invention was methodologically verified, and the performance index results are as follows.

[0136] 1. Linear relationship

[0137] Appropriate amounts of reference substances of liquiritin, hesperidin, honokiol, magnolol, costunolide, dehydrocostus lactone, and atractylodesin were accurately weighed and prepared into a series of reference substance solutions of different concentrations by adding methanol according to step 2 of Example 3. According to the chromatographic conditions of step 3 of Example 3, 1 μL of the reference substance solution was accurately aspirated and injected into the ultra-performance liquid chromatograph. A standard curve was plotted with the reference substance concentration (μg / mL) as the abscissa (x-axis) and the peak area of ​​each index component as the ordinate (y-axis). The quantification limit S / N was set to ≥10 and the detection limit S / N was set to ≥3. The standard regression equation, correlation coefficient, linear range, quantification limit, and detection limit of the multi-component were calculated. The specific results are shown in Table 2.

[0138] According to Table 2, the seven components have a good linear relationship within their respective injection mass concentration ranges, indicating that the method of the present invention has a wide linear range and high accuracy.

[0139] Table 2 Linear regression equation and correlation coefficient

[0140] 2. Stability

[0141] A sample of Zhengqi Tablets, batch number 200402, was taken and a test solution was prepared according to step 1 in Example 3. Samples were injected and analyzed at 0 h, 1 h, 3 h, 8 h, 12 h, and 24 h according to the chromatographic conditions of step 3 in Example 3. The chromatographic peak area data for liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin were recorded. The results showed that the RSDs of the chromatographic peak areas within 24 h were all less than 0.92%, indicating that the test solution had no effect on the results when tested within 24 h and had good stability.

[0142] 3. Precision

[0143] Take any reference solution prepared in step 2 of Example 3 and analyze it six times in a row using the chromatographic conditions of step 3 of Example 3. Record the peak area data for liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin. The results show that the RSD of the peak areas of the seven components for six consecutive injections was less than 0.32%, indicating good instrument precision.

[0144] 4. Repeatability

[0145] Six samples of Zhengqi Tablets (lot 200402) were accurately weighed and prepared in parallel according to step 1 in Example 3 to obtain six test solutions. The chromatographic conditions of step 3 in Example 3 were used for analysis. The peak areas of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol, and atractylodesin were recorded and their contents were calculated. The results showed that the RSDs for all seven components were less than 1.19%, indicating good reproducibility of the method.

[0146] 5. Spike recovery rate

[0147] Nine samples of Zhengqi Tablets (batch number 200402) of known concentration were weighed accurately, and three mass concentrations of low, medium, and high concentrations of any reference solution prepared in step 2 of Example 1 were added (equivalent to 50%, 100%, and 150% of the original mass fraction, respectively). Three portions of each mass concentration were taken and the test solution was prepared according to step 1 of Example 3. The samples were injected and analyzed according to the chromatographic conditions of step 3 of Example 3. The recovery rate and RSD of each component were calculated based on the measured amount and the added amount. The results are shown in Table 3. As shown in Table 3, the average recovery rate of the seven components was 94.44% to 104.24%, and the RSD was 1.08% to 2.80%, indicating that the accuracy of the method was good.

[0148] Table 3 Sample recovery test results (n=3)

[0149] Example 8

[0150] Ten batches of Zhengqi tablets samples of different batches were taken, and the test solutions were prepared according to step 1 in Example 3. The samples were injected and analyzed according to the chromatographic conditions of step 3 in Example 3, and the contents of liquiritin, hesperidin, honokiol, costunolide, dehydrocostus lactone, magnolol and atractylodesin were calculated respectively. The results are shown in Table 4.

[0151] As shown in Table 4, a total of 10 batches of Zhengqi tablets were tested using the established content determination method. According to the current quality standard, each tablet contains hesperidin (C 28 H 34 O 15) shall not be less than 0.8 mg. From the results in Table 4, we can see that all 10 batches of samples meet the requirements of the current standards.

[0152] Table 4 Sample content determination results

[0153] Example 9

[0154] The Zhengqi tablet sample 1# prepared in Example 1 and 10 reference substances were prepared according to step 1 in Example 3 to obtain test solution, and the chromatographic conditions of step 3 in Example 3 were followed. The results showed that the Zhengqi tablets could be qualitatively identified for 10 components, thereby better controlling the quality of the Zhengqi tablets. The specific results are shown in Figure 2. As shown in Figure 2, peak 1 is liquiritin, peak 2 is hesperidin, peak 3 is perilla ketone, peak 4 is nobiletin, peak 5 is tangeretin, peak 6 is honokiol, peak 7 is costunolide, peak 8 is dehydrocostus lactone, peak 9 is magnolol, and peak 10 is atractylodesin. Among them, perillone and tangeretin (peak 3 and peak 5) do not meet the general content requirements (≥0.02%) and are not suitable as quantitative indicators because their peak areas are too small and their contents are too low. At the same time, according to the provisions of the "Chinese Pharmacopoeia", when quantifying, the separation between the chromatographic peak of the substance to be measured and the adjacent chromatographic peaks should be greater than 1.5. Perillone, nobiletin and tangeretin (peak 3, peak 4, peak 5) do not meet this requirement, so they can only be qualitative.

[0155] In summary, the present invention provides a Zhengqi tablet, its preparation process, and a multi-component quantitative and qualitative assay method therein, capable of rapidly qualitatively analyzing 10 components in Zhengqi tablets and rapidly quantifying 7 of them. These methods offer simple operation, shortened assay time, excellent linearity, good repeatability, good precision, high accuracy, and excellent stability. Therefore, the present invention effectively overcomes the shortcomings of the prior art and possesses high industrial value.

[0156] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Anyone skilled in the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by one of ordinary skill in the art without departing from the spirit and technical principles disclosed herein are intended to be covered by the claims of the present invention.

Claims

1. A positive energy tablet, comprising the following components in parts by mass: Patchouli oil 0.5-1.5 parts; 0.1-1 part of perilla leaf oil; 150-250 parts of costus root; Atractylodes lancea 100-150 parts; Licorice 10-100 parts; 150-250 parts of Poria cocos; 100-150 parts of dried tangerine peel; 100-150 portions of processed Pinellia tuber; 100-150 parts of ginger magnolia bark; 100-150 servings of ginger.

2. The positive energy sheet according to claim 1, characterized in that: Calculated by mass, it includes the following components: Patchouli oil 0.8-1.2 parts; 0.4-0.8 parts of perilla leaf oil; 180-220 parts of costus root; Atractylodes lancea 130-140 parts; 60-70 parts of liquorice; Poria 180-220 parts; 130-140 parts of dried tangerine peel; 130-140 servings of processed pinellia tuber; 130-140 parts of ginger and magnolia bark; 130-140 servings of ginger.

3. The preparation process of the positive energy tablet according to any one of claims 1-2 comprises the following steps: 1) mixing the first part of costusroot, atractylodes and liquorice according to the proportion, crushing them into powder, and sieving to obtain material powder; 2) boiling the second part of Poria cocos, dried orange peel, processed Pinellia tuber, Magnolia officinalis bark, ginger, and licorice in water according to the proportion, filtering and concentrating the decoction to obtain a paste; 3) Mix the paste and powder and granulate them, then add patchouli oil and perilla leaf oil according to the proportion and press them into tablets.

4. The preparation process of the positive energy tablet according to claim 3, characterized in that: Includes any one or more of the following conditions: A1) in step 1) or 2), the mass ratio of the first part of licorice to the second part of licorice is 55-65:35-45; A2) In step 1), sucrose is also added during the mixing; preferably, the mass ratio of sucrose to costus root is 25-30:150-250; A3) In step 1), the mesh size of the sieve is 80-120 mesh; A4) in step 2), the decocting is performed until boiling; A5) In step 2), the decocting step is performed at least twice; A6) In step 2), the concentration temperature is 50-70°C; A7) in step 2), the concentration is performed to a relative density of 1.03-1.05; A8) In step 3), when the paste and powder are mixed, an appropriate amount of water is added to the paste; A9) In step 3), when the patchouli oil and perilla leaf oil are added, a lubricant is also added; preferably, the lubricant is talcum powder, and the amount of the lubricant added is 1.5-2.5% of the weight of the particles.

5. A positive energy tablet, prepared by the preparation process of the positive energy tablet according to any one of claims 3-4.

6. A method for quantitatively and qualitatively determining multiple components in Zhengqi tablets, comprising: The Zhengqi tablets described in any one of claims 1-2 and / or the Zhengqi tablets described in claim 4 are dissolved in methanol, then ultrasonically extracted and cooled. The supernatant is filtered and the obtained test solution is detected by ultra-performance liquid chromatography to qualitatively determine the contents of 10 components in the test solution: liquiritin, hesperidin, honokiol, costusin, dehydrocostusin, magnolol, atractylodesin, perillone, nobiletin and tangeretin; and quantitatively determine the contents of 7 components in the test solution: liquiritin, hesperidin, honokiol, costusin, dehydrocostusin, magnolol and atractylodesin.

7. The method for quantitatively and qualitatively determining multiple components in Zhengqi Tablets according to claim 6, characterized in that: Includes any one or more of the following conditions: B1) the ratio of the mass of the Zhengqi tablets added to the volume of the methanol added is 0.3:15-25, g / mL; B2) the ultrasonic extraction time is 30-60 minutes; B3) the power of the ultrasonic extraction is 200-350W; the frequency of the ultrasonic extraction is 40-60kHz; B4) cooling to room temperature; B5) The filtration is to take the supernatant through a filter membrane; preferably, the filter membrane is a 0.22 μm filter membrane.

8. The method for quantitatively and qualitatively determining multiple components in Zhengqi Tablets according to claim 6, characterized in that: The detection by ultra-high performance liquid chromatography comprises the following steps: A) Preparation of reference substance solution: adding methanol to dissolve the reference substances of liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin and tangeretin and making up to volume to prepare reference substance solution; B) Sample testing: Use ultra-high performance liquid chromatography to test the test solution and the reference solution in step A). The retention times were compared for qualitative analysis, and the external standard method was used for quantitative analysis. The contents of 10 components in the test solution were qualitatively determined: liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol, atractylodesin, perillone, nobiletin and tangeretin. The contents of 7 components in the test solution were quantitatively determined: liquiritin, hesperidin, honokiol, costunolide, dehydrocostuslactone, magnolol and atractylodesin.

9. The method for quantitatively and qualitatively determining multiple components in Zhengqi Tablets according to claim 8, characterized in that: The chromatographic conditions of the ultra-high performance liquid chromatography in step B) include any one or more of the following conditions: C1) The detector is a diode array detector; C2) the chromatographic column is a T3 chromatographic column; preferably, the chromatographic column is a Waters Acquity UPLC HSS T3 chromatographic column; C3) The detection wavelength is 224-226nm; C4) Column temperature is 30-45°C; C5) flow rate is 0.1-0.3 mL / min; C6) injection volume is 0.5 to 5 μL; C7) The mobile phase is acetonitrile-0.05-0.15% formic acid aqueous solution, wherein phase A is acetonitrile and phase B is 0.05-0.15% formic acid aqueous solution; the analysis time is 19 min; gradient elution.

10. The method for quantitatively and qualitatively determining multiple components in Zhengqi Tablets according to claim 9, characterized in that: C7), the specific procedure of the gradient elution is: 0-4min, the volume ratio of phase A:phase B was 20:80-35:65; 4-5min, the volume ratio of phase A:phase B is 35:65-40:60; 5-6 min, the volume ratio of phase A:phase B is 40:60-55:45; 6-15min, the volume ratio of phase A:phase B is 55:45-60:40; 15-16 min, the volume ratio of phase A:phase B is 60:40-90:10; 16-19min, the volume ratio of phase A:phase B is 90:10-90:10.

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