A synchronous green extraction method of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza

By using a composite bio-based solvent of glycerol formaldehyde and levulinic acid combined with ultrasonic extraction technology, tanshinone B, tanshinone I, cryptotanshinone, and tanshinone IIA can be extracted simultaneously from Salvia miltiorrhiza, solving the problems of low extraction efficiency and environmental pollution of traditional methods and achieving efficient and green extraction.

CN119118970BActive Publication Date: 2025-11-25ANHUI MEDICAL UNIV +1
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Patent Information

Application Number
CN202410745639.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-11
Publication Date
2025-11-25
Estimated Expiration
2044-06-11

AI Technical Summary

Technical Problem

Existing technologies are insufficient for the simultaneous and efficient extraction of hydrophilic component salvianolic acid B and hydrophobic components tanshinone I, cryptotanshinone, and tanshinone IIA from Salvia miltiorrhiza, and traditional organic solvent extraction methods pollute the environment.

Method used

A composite bio-based solvent consisting of glycerol formaldehyde and levulinic acid in a certain ratio was used to simultaneously extract salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from Salvia miltiorrhiza using ultrasonic extraction. The liquid-solid ratio, ultrasonic extraction temperature, time, and power were optimized.

Benefits of technology

It improved the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA, reduced the amount of organic solvents used, and achieved green and efficient extraction.

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Abstract

The application discloses a synchronous green extraction method of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in Danshen, which comprises the following steps: crushing Danshen into powder, and adding a bio-based solvent to the Danshen powder for ultrasonic-assisted extraction. When the extraction solvent is glycerol formal / acetic propionic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15 mL / g, the ultrasonic extraction temperature is 35 DEG C, the ultrasonic extraction time is 30 min, and the ultrasonic power is 360 W, the extraction rate of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in Danshen is 85.18 (mg / g), 0.347 (mg / g), 1.120 (mg / g) and 0.931 (mg / g) respectively, which is significantly higher than that of traditional methanol and ethanol. Therefore, the method provided by the application can effectively improve the extraction efficiency of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in Danshen, avoid the use of organic solvents such as methanol and ethanol, and is more green and environment-friendly.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of green process chemistry, and in particular to a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Danshen medicinal materials. BACKGROUND

[0002] Danshen is the dried root and rhizome of the Salvia miltiorrhiza Bge. of the Labiatae family, and has been used as a widely used traditional Chinese medicine for nearly 2000 years. It has the effects of activating blood and removing stasis, dredging channels and relieving pain, clearing the heart and relieving restlessness, and cooling blood and resolving abscesses. Salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are the main active components of Danshen, and are used as quality control indicators in the 2020 edition of the People's Republic of China Pharmacopoeia (Part I). Salvianolic acid B is a hydrophilic component with a high content in Danshen, and has good clinical efficacy for cardiovascular and cerebrovascular diseases, liver diseases, etc. Tanshinones are hydrophobic components, mainly including cryptotanshinone, tanshinone IIA and tanshinone I. Cryptotanshinone is the main anticancer active component, tanshinone IIA has obvious anti-inflammatory, antioxidant and antitumor activities, and tanshinone I is one of the bacteriostatic effective components of Danshen, and can treat acne and angina pectoris, and has the effects of improving lung inflammation and protecting nerves, etc.

[0003] Current natural product production mainly uses volatile organic solvents, which is low in efficiency and pollutes the environment. In addition, these organic solvent-based extraction methods can usually only target hydrophilic components or hydrophobic components, and it is difficult to simultaneously consider the efficient extraction of both types of components. It is of great significance to find a new type of solvent that is more green, has large-scale production potential, and can simultaneously and efficiently extract hydrophilic and hydrophobic components. Bio-based solvents are solvents converted from biomass, which are more green and efficient than volatile organic solvents. At present, there is still a lack of systematic research on the use of bio-based solvents to simultaneously and efficiently extract hydrophilic and hydrophobic natural products, especially the use of bio-based solvents to simultaneously and efficiently extract salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Danshen has not been studied. SUMMARY

[0004] The present application aims to overcome the shortcomings of the prior art, and provides a novel composite bio-based solvent by reasonable design, and establishes a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Danshen.

[0005] The present application provides a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Danshen, which comprises the following steps:

[0006] Step 1: providing a Danshen raw material, crushing to obtain Danshen powder;

[0007] Step two, providing an extraction solvent; the extraction solvent is a composite solvent composed of glycerol formaldehyde and levulinic acid in a certain proportion;

[0008] Step three, mixing the extraction solvent and the Danshen powder in a mass ratio of (5-45):1, and ultrasonic extraction at 120-600W to obtain an extracted mixture; the ultrasonic extraction temperature is 25-65℃, and the ultrasonic extraction time is 5-60min;

[0009] Step four, centrifuging the extracted mixture, taking the supernatant, and obtaining a Danshen extract

[0010] Optionally, the extraction solvent includes at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formaldehyde, ethyl lactate, γ-valerolactone, and a composite solvent composed of the above solvents.

[0011] Preferably, the extraction solvent is a composite solvent composed of glycerol formaldehyde and levulinic acid.

[0012] Preferably, the volume ratio of the extraction solvent glycerol formaldehyde and levulinic acid is 57.8 / 42.2.

[0013] Preferably, the extraction solvent and the Danshen powder are mixed in a ratio of 15:1 (mL / g).

[0014] Preferably, the ultrasonic extraction temperature is 35℃.

[0015] Preferably, the ultrasonic extraction time is 30min.

[0016] Preferably, the ultrasonic power is 360W.

[0017] Preferably, the extraction solvent and the Danshen powder are mixed in a ratio of 15:1 (mL / g) and ultrasonic extraction; the ultrasonic power is 360W; the ultrasonic extraction time is 30min, and the extraction agent is glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v).

[0018] The embodiment of the present application provides a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials, adopts pure water, carbonic acid glycerin ester, ethylene glycol, levulinic acid, glycerol formaldehyde, ethyl lactate, gamma-valerolactone and a composite solvent composed of the above solvents as an extraction solvent, extracts salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza powder by ultrasonic extraction, the optional range of liquid-solid ratio is (5-45):1 (mL / g), preferably 15:1 (mL / g), the optional range of the extraction solvent is any proportion composite of the extraction agent, preferably the extraction solvent is glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v). The optional range of ultrasonic extraction power is 120-600 W, preferably 360 W. The optional range of ultrasonic extraction temperature is 25-65 DEG C, preferably 35 DEG C. The optional range of ultrasonic extraction time is 5-60 min, preferably 30 min; the synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials is provided in the embodiment of the present application, when the extraction solvent is glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15:1 (mL / g), the ultrasonic extraction temperature is 35 DEG C, the ultrasonic extraction time is 30 min, and the ultrasonic power is 360 W, the extraction rate of salvianolic acid B from salvia miltiorrhiza is 85.17 (mg / g), the extraction rate of tanshinone I is 0.347 (mg / g), the extraction rate of cryptotanshinone is 1.120 (mg / g), and the extraction rate of tanshinone IIA is 0.931 (mg / g). Therefore, the synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials provided by the present application can effectively improve the extraction rate and reduce the amount of organic solvent used in the extraction process, and the extraction operation is simpler. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the present application, the following will briefly introduce the drawings needed to be used in the embodiments. Obviously, for those skilled in the art, other drawings can also be obtained from these drawings without any creative labor.

[0020] Figure 1 The flow chart of the synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to the embodiment 1 of the present application is shown;

[0021] Figure 2 The flow chart of the synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to the embodiment 2 of the present application is shown;

[0022] Figure 3This is a flowchart of a simultaneous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Salvia miltiorrhiza according to Example 3 of this application;

[0023] Figure 4 This is a flowchart of a simultaneous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Salvia miltiorrhiza according to Example 4 of this application;

[0024] Figure 5 This is a flowchart of a simultaneous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Salvia miltiorrhiza according to Example 5 of this application;

[0025] Figure 6 This is a flowchart of a simultaneous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Salvia miltiorrhiza according to Example 6 of this application; Detailed Implementation

[0026] Example 1

[0027] like Figure 1 As shown in the embodiments of this application, a simultaneous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from Salvia miltiorrhiza is provided, comprising the following steps:

[0028] Step S11: Provide a raw material of Salvia miltiorrhiza, pulverize it to obtain Salvia miltiorrhiza powder;

[0029] Specifically, the Danshen medicinal material is dried, crushed using a pulverizer, sieved, and the sieved Danshen powder is collected.

[0030] Step S12: Provide an extraction solvent, which is a mixture of biologically derived solvents in a certain proportion;

[0031] According to the methods described in the Chinese Pharmacopoeia, the extraction of tanshinone and salvianolic acid often employs organic reagents, such as methanol or 80% methanol. In this application, a composite solvent consisting of at least one of pure water, glyceryl carbonate, ethylene glycol, levulinic acid, glyceryl formal, ethyl lactate, and γ-valerol is mixed in a specific ratio and stirred manually or magnetically to obtain the extraction solvent.

[0032] Step S13: Mix the extraction solvent and the danshen powder at a mass ratio of (5-45):1, and perform ultrasonic extraction at 120-600W to obtain the extracted mixture; the ultrasonic extraction temperature is 25-65℃, and the ultrasonic extraction time is 5-60min.

[0033] The ultrasonic wave uses the strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, crushing and stirring effect of ultrasonic wave radiation pressure, increases the frequency and speed of molecular motion of the material, increases the penetration of the solvent, thereby accelerating the target component into the solvent and promoting the extraction process.

[0034] In step three, the extraction solvent obtained in step two and the salvia miltiorrhiza powder obtained in step one are mixed according to a certain mass ratio, i.e., a liquid-solid ratio, and then extraction is carried out under ultrasonic conditions. The liquid-solid ratio, extraction temperature, extraction time and ultrasonic power are important factors affecting the extraction rate. In the method provided in the embodiments of the present application, the liquid-solid ratio is limited to the range of (5-45):1, the ultrasonic extraction temperature is limited to the range of 25-65℃, the ultrasonic extraction time is limited to the range of 5-60min, and the ultrasonic power is limited to 120-600W. A higher extraction rate can be achieved, and the amount of organic solvent used in the extraction process can be reduced.

[0035] Step S14, centrifuging the mixture after extraction to obtain salvia miltiorrhiza extract;

[0036] After ultrasonic extraction, the mixture after extraction is separated by centrifugation at 4000r / min for 10min to obtain salvia miltiorrhiza extract.

[0037] The specific embodiments and beneficial effects of the method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza provided in the present application can be seen from the following examples.

[0038] Example 2

[0039] Please refer to Figure 2 The example 2 of the present application shows one possible implementation of the method provided in the present application. The extraction solvent of the example 2 includes at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formaldehyde, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents. The obtained extraction solvent is then used for ultrasonic extraction of salvia miltiorrhiza powder. Specifically:

[0040] Step S21, providing a salvia miltiorrhiza raw material, pretreating to obtain salvia miltiorrhiza powder;

[0041] Step S22, providing an extraction solvent; the extraction solvent includes at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formaldehyde, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents;

[0042] Step S23, taking 5 identical centrifuge tubes, adding equal mass of salvia miltiorrhiza powder into each centrifuge tube, and then adding the extraction solvent of step S22 into the centrifuge tubes according to a liquid-solid ratio of 15:1, respectively;

[0043] Step S24, the centrifugal tube obtained in step S23 is fixed in an ultrasonic cleaning instrument, and ultrasonic extraction is performed at room temperature for 30 min to obtain an extracted mixture;

[0044] It should be noted that in step S24, the power of the ultrasonic cleaning instrument is set to 300 W, and the frequency is set to 40 kHz.

[0045] Step S25, centrifuging the extracted mixture obtained in step S24 to obtain the supernatant to obtain an extract;

[0046] Step S26, the contents of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in the Danshen extract obtained in step S25 are determined by high performance liquid chromatography, and the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are calculated;

[0047] The extraction rate results of Example 2 are summarized and compared as shown in Table 1:

[0048] Table 1 Extraction rate of different extraction solvents

[0049]

[0050] As shown in Table 1, in Example 2, when pure water, ethylene glycol and levulinic acid are used as extraction solvents, the extraction rates of salvianolic acid B, tanshinone I and cryptotanshinone are higher. When glycerol formaldehyde is used as an extraction solvent, the extraction rate of tanshinone IIA is the highest.

[0051] Using ethylene glycol, levulinic acid and glycerol formaldehyde as extraction solvents, extraction is carried out in any proportion. The extraction rate results are summarized and compared as shown in Table 2:

[0052] Table 2

[0053]

[0054]

[0055] Glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v) is selected as the extraction solvent, and the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are the highest.

[0056] Example 3

[0057] Please refer to Figure 3 , the embodiment 3 of the present application is based on the steps described in the foregoing embodiment 2, which shows another possible implementation of the method provided by the present application. The essence is different from the foregoing embodiment. In embodiment 3, the Danshen powder is mixed with the extraction solvent at different liquid-solid ratios, and then ultrasonic extraction is carried out under the same conditions; specifically:

[0058] Step S31, providing a salvia miltiorrhiza raw material, pretreating to obtain a salvia miltiorrhiza powder;

[0059] Step S32, providing an extraction solvent; the extraction solvent is glycerol formal / acetic propionic acid (57.8 / 42.2, v / v);

[0060] Step S33, taking 5 identical centrifugal tubes, adding equal mass of salvia miltiorrhiza powder into each centrifugal tube, and then adding the extraction solvent of step S32 into the 5 centrifugal tubes respectively according to liquid-solid ratios of 5:1, 15:1, 25:1, 35:1 and 45:1;

[0061] Step S34, fixing the centrifugal tubes obtained in step S33 in an ultrasonic cleaning instrument, and ultrasonically extracting at room temperature for 30 min to obtain 5 kinds of extracted mixtures;

[0062] Step S35, centrifuging the 5 kinds of extracted mixtures obtained in step S34 to obtain 5 kinds of supernatants, and obtaining 5 kinds of extraction solutions;

[0063] Step S36, quantitatively determining the contents of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in the salvia miltiorrhiza extraction solution of step S35 by high performance liquid chromatography, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA;

[0064] The extraction rate results of example 3 are summarized and compared, as shown in table 3:

[0065] Table 3 extraction rates of different liquid-solid ratios

[0066]

[0067]

[0068] As shown in table 3, in example 3, when the liquid-solid ratio is 15:1, the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are the highest, reaching 74.90, 0.358, 1.059 and 0.872 respectively. Therefore, in the method provided by the present application, the liquid-solid ratio of 15:1 is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA.

[0069] Example 4

[0070] Please refer to Figure 4 , on the basis of the steps described in the foregoing examples 2 and 3, another possible implementation manner of the method provided by the present application is shown, which is different in essence from the foregoing examples. In example 4, after mixing the salvia miltiorrhiza powder with the extraction solvent, ultrasonic extraction is carried out under different extraction times, and other conditions are the same; specifically:

[0071] Step S41, providing a salvia miltiorrhiza raw material, pretreating to obtain a salvia miltiorrhiza powder;

[0072] Step S42, providing an extraction solvent; the extraction solvent is glycerol formal / acetic propionic acid (57.8 / 42.2, v / v);

[0073] Step S43, taking 5 identical centrifugal tubes, adding equal mass of salvia miltiorrhiza powder into each centrifugal tube, and adding the extraction solvent of step S42 into the 5 centrifugal tubes according to a liquid-solid ratio of 15:1;

[0074] Step S44, fixing the centrifugal tubes obtained in step S43 in an ultrasonic cleaning instrument, and ultrasonically extracting at room temperature for 5 min, 15 min, 30 min, 45 min and 60 min respectively under an ultrasonic power of 300 W, to obtain 5 kinds of extracted mixtures;

[0075] Step S45, centrifuging the 5 kinds of extracted mixtures obtained in step S44, and taking the supernatant to obtain 5 kinds of extraction solutions;

[0076] Step S46, quantitatively determining the contents of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in the salvia miltiorrhiza extraction solution of step S45 by high performance liquid chromatography, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA;

[0077] The extraction rate results of example 4 are summarized and compared, as shown in table 4:

[0078] Table 4 extraction rates at different extraction times

[0079]

[0080]

[0081] As shown in table 4, in example 4, when the extraction time is 30 min, the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are the highest, reaching 75.98, 0.366, 1.059 and 0.883 respectively. Therefore, in the method provided in the application, the extraction time is preferably 30 min, which is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA.

[0082] Example 5

[0083] Please refer to Figure 5Embodiment 5 of the present application is based on the steps described in the foregoing embodiments 2-4, and shows another possible implementation of the method provided by the present application. The difference between the present embodiment and the foregoing embodiments is that, in the present embodiment, the Danshen powder is mixed with the extraction solvent, and then ultrasonic extraction is performed at different extraction temperatures, with other conditions being the same. Specifically:

[0084] Step S51: providing a Danshen raw material, pretreating, and obtaining Danshen powder;

[0085] Step S52: providing an extraction solvent; the extraction solvent is glycerol formal / acetic propionic acid (57.8 / 42.2, v / v);

[0086] Step S53: taking 5 identical centrifuge tubes, adding an equal mass of Danshen powder into each centrifuge tube, and adding the extraction solvent of step S52 into the 5 centrifuge tubes according to a liquid-solid ratio of 15:1;

[0087] Step S54: fixing the centrifuge tubes obtained in step S53 in an ultrasonic cleaning instrument, and performing ultrasonic extraction at 25℃, 35℃, 45℃, 55℃, and 65℃ for 30 min, respectively, to obtain 5 kinds of extracted mixtures;

[0088] Step S55: centrifuging the 5 kinds of extracted mixtures obtained in step S54, and taking the supernatant to obtain 5 kinds of extraction solutions;

[0089] Step S56: quantitatively determining the contents of salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA in the Danshen extraction solution of step S55 by high performance liquid chromatography, and calculating the extraction rates of salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA;

[0090] The extraction rate results of embodiment 5 are summarized and compared, as shown in Table 5:

[0091] Table 5: extraction rates at different temperatures

[0092]

[0093] As shown in Table 5, in embodiment 5, when the extraction temperature is 35℃, the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA are the highest, reaching 76.11, 0.385, 1.054, and 0.907, respectively. Therefore, in the method provided by the present application, the preferred extraction temperature is 35℃, which is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA.

[0094] Embodiment 6

[0095] Please refer to Figure 6Embodiment 6 of the present application is based on the steps described in the foregoing embodiments 2-5, and shows another possible implementation of the method provided by the present application. The difference between the present embodiment and the foregoing embodiments is that, in the present embodiment, the Danshen powder is mixed with the extraction solvent, and then ultrasonic extraction is performed at different ultrasonic powers, with other conditions being the same. Specifically:

[0096] Step S61: providing a Danshen raw material, pretreating, and obtaining Danshen powder;

[0097] Step S62: providing an extraction solvent; the extraction solvent is glycerol formal / acetic propionic acid (57.8 / 42.2, v / v);

[0098] Step S63: taking 5 identical centrifuge tubes, adding an equal mass of Danshen powder into each centrifuge tube, and adding the extraction solvent of step S62 into the 5 centrifuge tubes according to a liquid-solid ratio of 15:1;

[0099] Step S64: fixing the centrifuge tubes obtained in step S63 in an ultrasonic cleaning instrument, and performing ultrasonic extraction at room temperature for 30 min at ultrasonic powers of 120 W, 240 W, 360 W, 480 W, and 600 W, respectively, to obtain 5 kinds of extracted mixtures;

[0100] Step S65: centrifuging the 5 kinds of extracted mixtures obtained in step S64, and taking the supernatant to obtain 5 kinds of extraction solutions;

[0101] Step S66: quantitatively determining the contents of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA in the Danshen extraction solution of step S65 by high performance liquid chromatography, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA;

[0102] The extraction rate results of embodiment 6 are summarized and compared, as shown in Table 6:

[0103] Table 6: extraction rates at different ultrasonic powers

[0104]

[0105] As shown in Table 6, in embodiment 6, when the ultrasonic power is 360 W, the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA are the highest, reaching 77.25, 0.377, 1.083, and 0.883, respectively. Therefore, in the method provided by the present application, the ultrasonic power is preferably 360 W, which is more conducive to improving the extraction rates of salvianolic acid, tanshinone I, cryptotanshinone, and tanshinone IIA.

[0106] The optimal conditions for extracting salvianolic acids, tanshinone I, tanshinone, tanshinone IIA were obtained when the extraction solvent was glycerol formal / acetic propionic acid (57.8 / 42.2, v / v), the liquid-solid ratio was 15:1, the ultrasonic extraction temperature was 35℃, the ultrasonic extraction time was 30 min, and the ultrasonic power was 360 W. Compared with the extraction method of salvianolic acids and tanshinones in the Chinese Pharmacopoeia, as shown in Table 7:

[0107] Table 7 Comparison of extraction methods

[0108]

[0109] a: glycerol formal / acetic propionic acid (57.8 / 42.2, v / v)

[0110] b: extraction method of salvianolic acids in the standard of Salvia miltiorrhiza in the Chinese Pharmacopoeia 2020 edition

[0111] c: extraction method of tanshinones in the standard of Salvia miltiorrhiza in the Chinese Pharmacopoeia 2020 edition

[0112] It can be seen that the method provided by the present application can significantly improve the extraction rate of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA extracted from Salvia miltiorrhiza.

[0113] The embodiment of the present application provides a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials, pure water, carbon glyceride, ethylene glycol, levulinic acid, glycerol formaldehyde, ethyl lactate and gamma-valerolactone are used as extraction solvents, salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are ultrasonically extracted from salvia miltiorrhiza powder, the optional range of liquid-solid ratio is (5-45):1, preferably 15:1, the optional range of extraction solvent is a composite solvent composed of glycerol formaldehyde and levulinic acid, preferably the extraction solvent is glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v). The optional range of ultrasonic extraction power is 120-600W, preferably 360W. The optional range of ultrasonic extraction temperature is 25-65℃, preferably 35℃. The optional range of ultrasonic extraction time is 5-60min, preferably 30min. The method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza is provided in the embodiment of the present application, when the extraction solvent is glycerol formaldehyde / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15:1, the ultrasonic extraction temperature is 35℃, the ultrasonic extraction time is 30min and the ultrasonic power is 360W, the extraction rate of salvianolic acid B extracted from salvia miltiorrhiza is 85.17 (mg / g), the extraction rate of tanshinone I is 0.347 (mg / g), the extraction rate of cryptotanshinone is 1.120 (mg / g) and the extraction rate of tanshinone IIA is 0.931 (mg / g). Therefore, the synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials provided in the present application can effectively improve the extraction rate, reduce the amount of organic solvent used in the extraction process and simplify the extraction operation.

[0114] The above-mentioned embodiments of the present application do not constitute a limitation on the protection scope of the present application.

Claims

1. A synchronous green extraction method of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in Danshen, characterized in that The steps are as follows: Step one, providing a salvia miltiorrhiza raw material, crushing to obtain salvia miltiorrhiza powder; Step two, providing an extraction solvent, the extraction solvent is a composite solvent composed of glycerol formaldehyde and acetylpic acid; Step three, the extraction solvent and the salvia miltiorrhiza powder are mixed according to the liquid-solid ratio of 5-45ml solvent per gram of powder, ultrasonic extraction is carried out at 120-600w to obtain the extracted mixture; the ultrasonic extraction temperature is 25-65℃, and the ultrasonic extraction time is 5-60min; Step four, centrifuging the extracted mixture, taking the supernatant to obtain salvia miltiorrhiza extract.

2. The method of claim 1, wherein, The volume ratio of glycerol formaldehyde to acetylpic acid in the extraction solvent is 57.8:42.

2.

3. The method of claim 1, wherein, The extraction solvent and the salvia miltiorrhiza powder are mixed according to the liquid-solid ratio of 15ml per gram.

4. The method of claim 1, wherein, The ultrasonic extraction temperature is 35℃.

5. The method of claim 1, wherein, The ultrasonic extraction time is 30min.

6. The method of claim 1, wherein, The ultrasonic power is 360w.

7. The method of claim 1, wherein, The extraction solvent and the salvia miltiorrhiza powder are mixed according to the liquid-solid ratio of 15ml per gram, ultrasonic extraction is carried out; the ultrasonic power is 360w; the volume ratio of glycerol formaldehyde to acetylpic acid in the extraction solvent is 57.8:42.2.

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