Steaming processing quality control method for traditional Chinese medicine rhizoma polygoni cuspidati

Abstract

The invention relates to the technical field of traditional Chinese medicines, and discloses a steaming processing quality control method of a traditional Chinese medicine rhizoma polygoni cuspidati, which comprises the following steps: mixing ginsenoside Ro, pseudoginsenoside RT1, panax japonicus saponin IV, panax japonicus saponin IVa, notoginsenoside R1, pseudo-ginsenoside RP1, calendula officinalis glycoside E, oleanolic acid beta-D-glucopyranosyl ester, ginsenoside RK1 and ethanol, stirring, filtering, and drying to obtain the traditional Chinese medicine rhizoma polygoni cuspidati. Obtaining a reference substance solution; grinding and sieving the rhizoma polygoni cuspidati steamed product, adding into ethanol, uniformly stirring, carrying out ultrasonic extraction, fixing the volume, centrifuging, and collecting supernate, so as to obtain a test solution; the reference solution and the test solution are injected into a high performance liquid chromatograph for content detection, the retention time RSD of the nine components is smaller than 0.66%, the peak area RSD of the nine components is smaller than 2.40%, and therefore the detection and analysis method has good precision.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicine, and in particular to a quality control method for the seven-steaming preparation of Chinese medicine buttons. Background Art

[0002] Knotweed, also known as pearl ginseng, large-leaf Panax notoginseng, button seven, knot seven, and pan seven, has high medicinal value. Among them, saponins, as the main medicinal ingredients of Knotweed, have a content of more than 65%. Pharmacological studies have shown that saponins have the effects of reducing the body's oxygen consumption, inhibiting platelet aggregation and increasing cerebral blood flow, lowering blood lipids and blood sugar, resisting fatigue, and improving macrophage function. They are important factors that determine the quality and efficacy of Knotweed. Therefore, it is necessary to strictly detect and control the indicators of saponins in Knotweed.

[0003] Processing refers to the process of making unprocessed Chinese medicinal materials of button seven into medicinal slices for clinical use through cleaning, cutting, frying, calcining, roasting, roasting, soaking, soaking, steaming and boiling under the guidance of traditional Chinese medicine theory. After processing, the material basis of button seven changes, which can significantly increase the saponin content. However, due to the lack of scientific and efficient quality standards for button seven, the efficacy is unstable and cannot fully reflect the overall quality of the medicinal materials. In addition, during the steaming and processing process of the Chinese medicinal materials of button seven, the starch contained in it is easily gelatinized, which wraps the saponin components in button seven and forms a physical barrier, resulting in a decrease in the saponin peak area during the measurement process, resulting in large errors. Summary of the Invention

[0004] The invention provides a quality control method for the steaming and processing of the traditional Chinese medicine Kouziqi, which solves the problem that Kouziqi lacks scientific and efficient quality specifications, resulting in unstable efficacy and inability to fully reflect the overall quality of the medicinal material.

[0005] The technical solution of the present invention:

[0006] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0007] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with ethanol and stirred to obtain a reference solution;

[0008] S2. Grind and sieve the steamed product of button seven, add it to ethanol, stir it evenly, extract it with ultrasound, make it up to volume, and collect the supernatant by centrifugation to obtain the test solution;

[0009] S3. Inject the reference solution and test solution into the high performance liquid chromatograph for content detection respectively.

[0010] Furthermore, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.2-1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.86-1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.76-0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.6-1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.43-0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.28-0.32 mg / mL, the concentration of calendulaside E is 1.83-1.85 mg / mL, the concentration of oleanolic acid β-D-pyranosyl ester is 0.08-0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.07-0.09 mg / mL.

[0011] Furthermore, in step S2, the ultrasonic extraction power is 350-370W, the ultrasonic extraction frequency is 30-50kHz, and the ultrasonic extraction time is 35-45min.

[0012] Further, in step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (0-7 min, mobile phase B is 30-32%; 7-10 min, mobile phase B is 32-35%; 10-12 min, mobile phase B is 35-43%; 12-14 min, mobile phase B is 43-43%; 14-16 min, mobile phase B is 43-47%; 16-21 min, mobile phase B is 50-60%; 17-20 min, mobile phase B is 100-100%; 18-21 min, mobile phase B is 100-200%; 20-30 min, mobile phase B is 100-100%; 21-30 min, mobile phase B is 100-100%; 22-30 min, mobile phase B is 100-100%; 23-30 min, mobile phase B is 100-100%; 24-30 min, mobile phase B is 100-100%; 25-30 min, mobile phase B is 100-100%; 26-30 min, mobile phase B is 100-100%; 27-30 min, mobile phase B is 100-100%; 28-30 min, mobile phase B is 100-100%; 29-40 min, mobile phase B is 100-100%; 30-40 min, mobile phase B is 100-100% Mobile phase B is 47-54%; 21-22 min, mobile phase B is 54-54%; 22-23 min, mobile phase B is 54-56%; 23-24 min, mobile phase B is 56-56%; 24-30 min, mobile phase B is 56-70%; 30-35 min, mobile phase B is 70-30%); flow rate is 0.2-0.4 mL / min; detection wavelength is 200-206 nm; column temperature is 28-32°C; injection volume is 1 μL.

[0013] Furthermore, in step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw product medicinal materials, nanogel and water, stirring evenly, steaming, and drying to obtain the button seven steamed product;

[0014] The nanogel is obtained by mixing cellulase, α-amylase, β-glucosidase and calcium lactate to form a complex, which is then coated with hyaluronic acid and vitamin E.

[0015] Furthermore, the moistening temperature is 30-40° C., and the moistening time is 1-4 hours.

[0016] Furthermore, the steaming temperature is 115-130° C., and the steaming time is 1-4 hours; the drying temperature is 70-90° C., and the drying time is 5-10 minutes.

[0017] Furthermore, the mass ratio of the Kouziqi raw material, nanogel and water is (2-3):(0.5-0.7):(10-15).

[0018] Furthermore, the nanogel is specifically prepared by the following steps:

[0019] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 40-50°C for 20-30 minutes, and dried at room temperature overnight to obtain a complex;

[0020] A2. Add the complex to deionized water, stir evenly, add hyaluronic acid and vitamin E, stir at 40-50°C for 3-6 hours, stir at 1000-1500 r / min for 20-30 minutes, and dry at room temperature overnight to obtain a nanogel.

[0021] Furthermore, during the above-mentioned reaction A1, calcium ions in calcium lactate can combine with cellulase, α-amylase, and β-glucosidase to form a stable system.

[0022] Furthermore, during the above-mentioned A2 reaction, the carboxyl groups of hyaluronic acid and the hydroxyl groups of vitamin E condense under mild heating to form a cross-linked structure, and the complex enzyme can be embedded in the cross-linked structure to form a nanogel with a size of 500-600 nm and a gel pore size of 50-60 nm.

[0023] Furthermore, in step A1, the mass ratio of the cellulase, α-amylase, β-glucosidase, calcium lactate and deionized water is (1.4-1.6):(1.2-1.4):(1.1-1.3):(0.4-0.6):(18-22).

[0024] Furthermore, in step A2, the mass ratio of the complex, deionized water, hyaluronic acid and vitamin E is (3.6-4):(45-55):(5-7):(1-3).

[0025] The present invention has the following beneficial effects:

[0026] (1) In the technical solution of the present invention, a complex formed by mixing cellulase, α-amylase, β-glucosidase and calcium lactate is mixed with the button seven medicinal material for steaming and moistening. The cellulase can hydrolyze the cell wall (cellulose, hemicellulose) of the button seven medicinal material, destroy the cell wall and cell membrane structure of the button seven medicinal material, so that heat can more easily penetrate into the button seven medicinal material during steaming, shortening the steaming time, improving the processing efficiency, and making it easier to release the saponin components in the button seven medicinal material, thereby increasing the saponin dissolution rate and reducing the detection error.

[0027] (2) In the technical solution of the present invention, β-glucosidase can hydrolyze the released saponin glycoside chains, promote the conversion of native saponins into rare ginsenosides, and increase the content of rare saponins; α-amylase can specifically hydrolyze the glycosidic bonds in starch, decompose amylose and amylopectin into small molecular dextrins, maltose and glucose, destroy the macromolecular chain structure of starch, avoid the encapsulation of saponin components by starch gelatinization, increase the dissolution rate of saponins, and thus reduce detection errors.

[0028] (3) In the technical solution of the present invention, the calcium ions in calcium lactate can combine cellulase and β-glucosidase to form a temperature system, which is conducive to the cellulase breaking the wall to release saponin components, and β-glucosidase hydrolyzing saponin components into rare ginsenosides. In addition, the calcium ions can combine with the hydroxyl groups of starch in the button seven medicinal material, consume the hydroxyl groups of starch, inhibit the formation of a gel network after gelatinization, reduce the physical packaging of saponins, and improve the detection accuracy. As a food-grade agent, calcium lactate will not affect the efficacy of the button seven medicinal material.

[0029] (4) In the technical solution of the present invention, the complex is coated in hyaluronic acid and vitamin E to form a nanogel. On the one hand, the nanogel is evenly dispersed in water to form a nanofluid, which can better penetrate into the button seven medicinal materials, inhibiting starch gelatinization and increasing the content of rare saponins. On the other hand, the formed nanogel contains a porous structure and can effectively release the complex. In addition, vitamin E can combine with free radicals to prevent the oxidative degradation of saponins, thereby improving the detection accuracy. Hyaluronic acid contains a large number of carboxyl groups, which can also consume the hydroxyl groups of starch, inhibiting the formation of a gel network after its gelatinization, reducing the physical packaging of saponins, and improving the detection accuracy.

[0030] (5) In the technical solution of the present invention, the reference solution and the test solution were respectively injected into the high performance liquid chromatograph for content detection. The retention time RSDs of the nine components in the reference solution and the test solution were recorded to be less than 0.66%, and the peak area RSDs were less than 2.40%, indicating that the detection and analysis method of the present invention has good precision. DETAILED DESCRIPTION

[0031] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0032] The raw materials used in the examples of the present invention are as follows, and all reagents used are of analytical grade.

[0033] Among them, the raw medicinal material of Kouziqi was identified by Associate Professor Gong Limin of Hunan University of Chinese Medicine as the dried rhizome of P.japonicus CAMey.var.bipinnatifidus(Seem.)CYWu et KMFeng.

[0034] Cellulase model X12433 was purchased from Hangzhou Xiaoyou Biotechnology Co., Ltd.; α-amylase model YN was purchased from Jinan Yunuo Chemical Co., Ltd.; β-glucosidase EINECS number 232-589-7 was purchased from Shenzhen Lefu Biotechnology Co., Ltd.

[0035] Vitamin E was purchased from Shaanxi Taike Biotechnology Co., Ltd.

[0036] Example 1

[0037] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0038] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0039] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract under ultrasonication at 350 W, 30 kHz for 35 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0040] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0041] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.2 mg / mL, the concentration of pseudoginsenoside RT1 is 1.86 mg / mL, the concentration of bamboo ginsenoside IV is 0.76 mg / mL, the concentration of bamboo ginsenoside IVa is 1.6 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.43 mg / mL, the concentration of pseudoginsenoside RP1 is 0.28 mg / mL, the concentration of calendulaside E is 1.83 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.08 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.07 mg / mL;

[0042] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid (A); acetonitrile (B), gradient elution (0 min, mobile phase A is 70%, mobile phase B is 30%; 7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 57%, mobile phase B is 43%; Mobile phase A is 53%, mobile phase B is 47%; 21 min, mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%); flow rate is 0.2 mL / min; detection wavelength is 200 nm; column temperature is 28°C; injection volume is 1 μL.

[0043] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 30°C for 1 hour, steaming at 115°C for 1 hour, and drying at 70°C for 5 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 2:0.5:10.

[0044] In step S2, the nanogel is specifically prepared by the following steps:

[0045] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 40°C for 20 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.4:1.2:1.1:0.4:18;

[0046] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 40°C for 3 hours, then at 1000 rpm for 20 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 3.6:45:5:1.

[0047] Example 2

[0048] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0049] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0050] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 360 W, 40 kHz for 40 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0051] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0052] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.22 mg / mL, the concentration of pseudoginsenoside RT1 is 1.87 mg / mL, the concentration of bamboo ginsenoside IV is 0.77 mg / mL, the concentration of bamboo ginsenoside IVa is 1.62 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.44 mg / mL, the concentration of pseudoginsenoside RP1 is 0.30 mg / mL, the concentration of calendulaside E is 1.84 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.10 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.08 mg / mL;

[0053] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid (A); acetonitrile (B), gradient elution (5 min, mobile phase A is 69%, mobile phase B is 31%; 8 min, mobile phase A is 66%, mobile phase B is 34%; 11 min, mobile phase A is 60%, mobile phase B is 40%; 13 min, mobile phase A is 57%, mobile phase B is 43%; 15 min, mobile phase A is 55%, mobile phase B is 45%; 18 min, mobile phase A is 50%, mobile phase B is 50%, mobile phase B is 50%, mobile phase B is 50%, mobile phase A ... Mobile phase A is 50%, mobile phase B is 50%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 45%, mobile phase B is 55% B; 23 min, mobile phase A is 44%, mobile phase B is 56% B; 28 min, mobile phase A is 35%, mobile phase B is 65%; 33 min, mobile phase A is 50%, mobile phase B is 50%); flow rate is 0.3 mL / min; detection wavelength is 203 nm; column temperature is 30°C; injection volume is 1 μL.

[0054] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 35°C for 2.5 hours, steaming at 125°C for 2 hours, and drying at 80°C for 8 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 2.5:0.6:13.

[0055] In step S2, the nanogel is specifically prepared by the following steps:

[0056] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 45°C for 25 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.5:1.3:1.2:0.5:20;

[0057] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 45°C for 5 hours, then at 1300 rpm for 25 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 3.8:50:6:2.

[0058] Example 3

[0059] A method for controlling the quality of a traditional Chinese medicine prepared by steaming seven times, comprising the following steps:

[0060] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0061] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0062] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0063] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0064] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0065] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0066] In step S2, the nanogel is specifically prepared by the following steps:

[0067] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.6:1.4:1.3:0.6:22;

[0068] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 50°C for 6 hours, then at 1500 rpm for 30 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 4:55:7:3.

[0069] Comparative Example 1

[0070] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0071] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0072] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0073] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0074] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0075] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0076] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0077] In step S2, the nanogel is specifically prepared by the following steps:

[0078] A1. α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.4:1.3:0.6:22;

[0079] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 50°C for 6 hours, then at 1500 rpm for 30 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 4:55:7:3.

[0080] Comparative Example 2

[0081] A method for controlling the quality of a traditional Chinese medicine prepared by steaming seven times, comprising the following steps:

[0082] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0083] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0084] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0085] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0086] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0087] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0088] In step S2, the nanogel is specifically prepared by the following steps:

[0089] A1. Cellulase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, β-glucosidase, calcium lactate, and deionized water was 1.6:1.3:0.6:22;

[0090] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 50°C for 6 hours, then at 1500 rpm for 30 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 4:55:7:3.

[0091] Comparative Example 3

[0092] A method for controlling the quality of a traditional Chinese medicine prepared by steaming seven times, comprising the following steps:

[0093] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0094] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0095] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0096] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0097] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0098] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0099] In step S2, the nanogel is specifically prepared by the following steps:

[0100] A1. Cellulase, α-amylase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, calcium lactate, and deionized water was 1.6:1.4:0.6:22;

[0101] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 50°C for 6 hours, then at 1500 rpm for 30 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 4:55:7:3.

[0102] Comparative Example 4

[0103] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0104] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0105] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0106] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0107] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0108] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0109] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0110] In step S2, the nanogel is specifically prepared by the following steps:

[0111] A1. Cellulase, α-amylase, and β-glucosidase were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, and deionized water was 1.6:1.4:1.3:22;

[0112] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were then added. The mixture was stirred at 50°C for 6 hours, then at 1500 rpm for 30 minutes, and dried overnight at room temperature to obtain a nanogel. The mass ratio of the complex, deionized water, hyaluronic acid, and vitamin E was 4:55:7:3.

[0113] Comparative Example 5

[0114] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0115] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0116] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0117] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0118] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0119] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0120] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0121] In step S2, the nanogel is specifically prepared by the following steps:

[0122] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.6:1.4:1.3:0.6:22;

[0123] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid was added and stirred at 50°C for 6 hours, at 1500 rpm for 30 minutes, and dried at room temperature overnight to obtain a nanogel; wherein the mass ratio of the complex, deionized water, and hyaluronic acid was 4:55:10.

[0124] Comparative Example 6

[0125] A method for controlling the quality of a traditional Chinese medicine button seven-steaming process comprises the following steps:

[0126] S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with 60% ethanol and stirred to obtain a reference solution;

[0127] S2. Grind 1 g of steamed kouziqi product, pass it through a 40-mesh sieve, and add it to 50 mL of 60% ethanol. Stir and extract it ultrasonically at 370 W and 50 kHz for 45 min. Add 60% ethanol to make the volume 50 mL. Centrifuge at 13,000 rpm for 10 min and collect the supernatant to obtain the test solution.

[0128] S3. The reference solution and the test solution were injected into the high performance liquid chromatograph for content detection;

[0129] Wherein, in step S1, the concentration of ginsenoside Ro in the reference solution is 1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.32 mg / mL, the concentration of calendulaside E is 1.85 mg / mL, the concentration of β-D-glucopyranosyl oleanolic acid ester is 0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.09 mg / mL;

[0130] In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (7 min, mobile phase A is 68%, mobile phase B is 32%; 10 min, mobile phase A is 65%, mobile phase B is 35%; 12 min, mobile phase A is 57%, mobile phase B is 43%; 14 min, mobile phase A is 57%, mobile phase B is 43%; 16 min, mobile phase A is 53%, mobile phase B is 47%; 21 min, Mobile phase A is 46%, mobile phase B is 54%; 22 min, mobile phase A is 46%, mobile phase B is 54%; 23 min, mobile phase A is 44%, mobile phase B is 56%; 24 min, mobile phase A is 44%, mobile phase B is 56%; 30 min, mobile phase A is 30%, mobile phase B is 70%; 35 min, mobile phase A is 70%, mobile phase B is 30%); flow rate is 0.4 mL / min; detection wavelength is 206 nm; column temperature is 32°C; injection volume is 1 μL.

[0131] In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw medicinal materials, nanogel and water, stirring evenly, steaming at 40°C for 4 hours, steaming at 130°C for 4 hours, and drying at 90°C for 10 minutes to obtain the button seven steamed product; wherein the mass ratio of the button seven raw medicinal materials, nanogel and water is 3:0.7:15.

[0132] In step S2, the nanogel is specifically prepared by the following steps:

[0133] A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 50°C for 30 minutes, and dried at room temperature overnight to obtain a complex; wherein the mass ratio of cellulase, α-amylase, β-glucosidase, calcium lactate, and deionized water was 1.6:1.4:1.3:0.6:22;

[0134] A2. The complex was added to deionized water and stirred evenly. Hyaluronic acid and vitamin E were added, and the mixture was stirred at 50°C for 6 hours, at 1500 rpm for 30 minutes, and dried at room temperature overnight to obtain a nanogel; wherein the mass ratio of the complex, deionized water, and vitamin E was 4:55:10.

[0135] The content of saponins in the steamed Kouziqi product was detected using the quality control method for steaming Kouziqi in Examples 1-3 and Comparative Examples 1-6.

[0136] The reference solution was injected and analyzed according to the above chromatographic conditions. The standard curve was drawn with the concentration of each reference substance as the horizontal axis (X) and the peak area value as the vertical axis (Y). The linear relationship of the correlation coefficient (r) was calculated. The results are shown in Table 1.

[0137] Table 1 Regression equations and linear ranges of nine components

[0138]

[0139] The reference solution and the test solution were respectively injected into a high performance liquid chromatograph for content detection, and the retention time RSDs of the nine components in the reference solution and the test solution were recorded to be less than 0.66%, and the peak area RSDs were less than 2.40%, indicating that the detection and analysis method of the present invention has good precision.

[0140] Take the raw product of Kouziqi and the steamed product of Kouziqi and prepare them into raw product test sample solution and steamed product test sample solution according to the above method, and then use the chromatographic conditions in the above detection method to determine the content of the nine components; ND means that no saponin components were detected.

[0141] The test results are shown in Table 2 below.

[0142] Table 2 Determination results of the contents of 9 ingredients in Examples 1-3 and Comparative Examples 1-6

[0143]

[0144]

[0145] It can be seen from the data in Table 1 that the content of saponin components in the steamed product of Kouziqi is detected by using a quality control method for steaming the Chinese medicine Kouziqi in Examples 1-3. The detection error is small, and the steamed product of Kouziqi prepared by the processing method of the present invention contains a large amount of rare saponin components.

[0146] In comparative example 1, no cellulase was added in step A1, no α-amylase was added in comparative example 2, no β-glucosidase was added in comparative example 3, and no calcium lactate was added in comparative example 4 to prepare the nanogel used to prepare the button seven medicinal materials, and then the detection method of the present invention was used for detection. The detection error was large, which proved that cellulase, α-amylase, β-glucosidase and calcium lactate can increase the saponin dissolution rate, and can avoid the encapsulation of saponin components by starch gelatinization, thereby increasing the dissolution rate of saponins and reducing the detection error.

[0147] In comparative example 5, only hyaluronic acid was used, and in comparative example 6, only vitamin E was used to prepare the nanogel for preparing the button seven medicinal materials. Then, the detection method of the present invention was used for detection. The detection error was large, which proved that the complex was coated in hyaluronic acid and vitamin E, and the formed nanogel penetrated better into the button seven medicinal materials, inhibiting starch gelatinization, increasing the content of rare saponins, and reducing the detection error.

[0148] Throughout the specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0149] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in similar ways. As long as they do not deviate from the invention or exceed the scope defined by the claims, they should all fall within the scope of protection of the present invention.

Claims

1. A method for controlling the quality of a traditional Chinese medicine button seven-steaming process, characterized in that: The following steps are involved: S1. Ginsenoside Ro, pseudoginsenoside RT1, bamboo ginsenoside IV, bamboo ginsenoside IVa, ginger-shaped notoginsenoside R1, pseudoginsenoside RP1, calendulaside E, oleanolic acid β-D-pyranosyl glucopyranose, ginsenoside RK1 were mixed with ethanol and stirred to obtain a reference solution; S2. Grind and sieve the steamed product of button seven, add it to ethanol, stir it evenly, extract it with ultrasound, make it up to volume, and collect the supernatant by centrifugation to obtain the test solution; S3. Inject the reference solution and test solution into the high performance liquid chromatograph for content detection respectively.

2. The method for controlling the quality of the steamed Chinese medicine Button Seven according to claim 1, wherein: In step S1, the concentration of ginsenoside Ro in the reference solution is 1.2-1.24 mg / mL, the concentration of pseudoginsenoside RT1 is 1.86-1.88 mg / mL, the concentration of bamboo ginsenoside IV is 0.76-0.78 mg / mL, the concentration of bamboo ginsenoside IVa is 1.6-1.64 mg / mL, the concentration of ginger-like notoginsengside R1 is 0.43-0.45 mg / mL, the concentration of pseudoginsenoside RP1 is 0.28-0.32 mg / mL, the concentration of calendulaside E is 1.83-1.85 mg / mL, the concentration of oleanolic acid β-D-pyranosyl glucopyranose is 0.08-0.12 mg / mL, and the concentration of ginsenoside RK1RT1 is 0.07-0.09 mg / mL.

3. The method for controlling the quality of the steamed Chinese medicine Button Seven according to claim 1, wherein: In step S2, the ultrasonic extraction power is 350-370 W, the ultrasonic extraction frequency is 30-50 kHz, and the ultrasonic extraction time is 35-45 min.

4. The method for controlling the quality of the steamed Chinese medicine Button Seven according to claim 1, wherein: In step S2, the button seven steamed product is specifically prepared by the following steps: mixing the button seven raw product medicinal materials, nanogel and water, stirring evenly, steaming, steaming and drying to obtain the button seven steamed product; The nanogel is obtained by mixing cellulase, α-amylase, β-glucosidase and calcium lactate to form a complex, which is then coated with hyaluronic acid and vitamin E.

5. The method for controlling the quality of the Chinese medicine button seven steaming process according to claim 4, wherein: The nanogel is specifically prepared by the following steps: A1. Cellulase, α-amylase, β-glucosidase, and calcium lactate were added to deionized water, stirred at 40-50°C for 20-30 minutes, and dried at room temperature overnight to obtain a complex; A2. Add the complex to deionized water, stir evenly, add hyaluronic acid and vitamin E, stir at 40-50°C for 3-6 hours, stir at 1000-1500 r / min for 20-30 minutes, and dry at room temperature overnight to obtain a nanogel.

6. The method for controlling the quality of the Chinese medicine button seven-steaming process according to claim 5, characterized in that: In step A1, the mass ratio of the cellulase, α-amylase, β-glucosidase, calcium lactate and deionized water is (1.4-1.6):(1.2-1.4):(1.1-1.3):(0.4-0.6):(18-22).

7. The method for controlling the quality of the Chinese medicine button seven-steaming process according to claim 5, characterized in that: In step A2, the mass ratio of the complex, deionized water, hyaluronic acid and vitamin E is (3.6-4):(45-55):(5-7):(1-3).

8. The method for controlling the quality of the traditional Chinese medicine button seven steaming process according to claim 4, characterized in that: The moistening temperature is 30-40° C., and the moistening time is 1-4 hours.

9. The method for controlling the quality of the Chinese medicine button seven steaming process according to claim 4, wherein: The steaming temperature is 115-130° C., and the steaming time is 1-4 hours; the drying temperature is 70-90° C., and the drying time is 5-10 minutes.

10. The method for controlling the quality of the traditional Chinese medicine Button Seven Steaming Process according to claim 1, characterized in that: In step S3, the chromatographic conditions are as follows: chromatographic column: Waters CORTECS UPLC T3 chromatographic column (2.1×100 mm, 1.6 μm), mobile phase: 0.1% phosphoric acid water (A); acetonitrile (B), gradient elution (0-7 min, mobile phase B is 30-32%; 7-10 min, mobile phase B is 32-35%; 10-12 min, mobile phase B is 35-43%; 12-14 min, mobile phase B is 43-43%; 14-16 min, mobile phase B is 43-47%; 16-21 min, mobile phase B is 47-54%; 21-22 min, mobile phase B is 54-54%; 22-23 min, mobile phase B is 54-56%; 23-24 min, mobile phase B is 56-56%; 24-30 min, mobile phase B is 56-70%; 30-35 min, mobile phase B is 70-30%); flow rate is 0.2-0.4 mL / min; detection wavelength is 200-206 nm; column temperature is 28-32°C; injection volume is 1 μL.

Images