Synchronous green extraction method for salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza

Abstract

The invention discloses a synchronous green extraction method for salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza, which comprises the following steps: crushing the salvia miltiorrhiza into powder, and adding a bio-based solvent into the salvia miltiorrhiza powder for ultrasonic-assisted extraction. According to the synchronous green extraction method of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza, provided by the embodiment of the invention, when the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15mL / g, the ultrasonic extraction temperature is 35 DEG C, the ultrasonic extraction time is 30min and the ultrasonic power is 360W, the content of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza can be effectively reduced, and the extraction efficiency is improved. The extraction rate of salvianolic acid is 85.18 (mg / g), the extraction rate of tanshinone I is 0.347 (mg / g), the extraction rate of tanshinone is 1.120 (mg / g), and the extraction rate of tanshinone IIA is 0.931 (mg / g), which are significantly higher than those of traditional methanol and ethanol. Therefore, according to the method provided by the invention, the salvianolic acid B, the tanshinone I, the cryptotanshinone and the tanshinone IIA are extracted from the radix salviae miltiorrhizae, the efficiency can be effectively improved, the use of organic solvents methanol and ethanol is avoided, and the method is more environment-friendly.

Description

Technical Field

[0001] The invention 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 salvia miltiorrhiza medicinal materials. Background Art

[0002] Danshen is the dried root and rhizome of Salvia miltiorrhiza Bge., a plant of the Lamiaceae family. As a widely used traditional Chinese medicine, it has a long history of nearly 2,000 years. It has the effects of promoting blood circulation and removing blood stasis, relieving pain by promoting menstruation, clearing the heart and relieving restlessness, cooling blood and eliminating carbuncle. Salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA are the main active ingredients of danshen, and are used as quality control indicators in the 2020 edition of the Pharmacopoeia of the People's Republic of China (Volume 1). Salvianolic acid B is a hydrophilic component with a high content in danshen, and has good clinical efficacy for cardiovascular and cerebrovascular diseases and liver diseases. Tanshinones are hydrophobic components, mainly including cryptotanshinone, tanshinone ⅡA, and tanshinone Ⅰ. Among them, cryptotanshinone is the main anti-cancer active ingredient, tanshinone ⅡA has obvious anti-inflammatory, antioxidant, and anti-tumor activities, and tanshinone Ⅰ is one of the antibacterial active ingredients of danshen, and can treat acne and angina pectoris, and has the effects of improving lung inflammation and protecting nerves.

[0003] At present, volatile organic solvents are mainly used in the production of natural products, which are inefficient and pollute the environment. In addition, these organic solvent-based extraction methods can usually only target hydrophilic components or hydrophobic components, and it is difficult to take into account the efficient extraction of both types of components at the same time. It is of great significance to find a new solvent that is greener, has the potential for large-scale production, and can efficiently extract hydrophilic and hydrophobic components at the same time. Bio-based solvents are solvents converted from biomass, which are greener and more efficient than volatile organic solvents. At present, there is still a lack of systematic research on the simultaneous and efficient extraction of hydrophilic and hydrophobic natural products using bio-based solvents, especially the simultaneous and efficient extraction of salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in Salvia miltiorrhiza using bio-based solvents. Summary of the invention

[0004] The purpose of the present invention is to obtain a new composite bio-based solvent through reasonable design to address the shortcomings of the existing methods, and to establish a synchronous green extraction method for salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza.

[0005] The present application embodiment provides a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza, comprising:

[0006] Step 1, providing a salvia miltiorrhiza raw material, crushing it to obtain salvia miltiorrhiza powder;

[0007] Step 2, providing an extraction solvent; the extraction solvent is a composite solvent composed of glycerol formal and levulinic acid in a certain proportion;

[0008] Step 3, mixing the extraction solvent and the Salvia miltiorrhiza powder in a mass ratio of (5-45):1, and ultrasonically extracting at 120-600W to obtain an extracted mixture; the temperature of the ultrasonic extraction is 25-65°C, and the time of the ultrasonic extraction is 5-60min;

[0009] Step 4: Centrifuge the extracted mixture and take the supernatant to obtain the Danshen extract.

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

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

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

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

[0014] Preferably, the temperature of the ultrasonic extraction is 35°C.

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

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

[0017] Preferably, the extraction solvent and Salvia miltiorrhiza powder are mixed in a ratio of 15:1 (mL / g) and ultrasonic extraction is performed; the ultrasonic power is 360 W; the ultrasonic extraction time is 30 min, wherein the extractant is glycerol formal / 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, using pure water, carbonate glycerol, ethylene glycol, levulinic acid, glycerol formal, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents as an extraction solvent, ultrasonically extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza powder, the liquid-solid ratio can be in the range of (5-45):1 (mL / g), preferably 15:1 (mL / g), the extraction solvent can be in the range of any ratio of the extractant, preferably the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v). The ultrasonic extraction power can be in the range of 120-600W, preferably 360W. The ultrasonic extraction temperature can be in the range of 25-65°C, preferably 35°C. The optional range of ultrasonic extraction time is 5-60min, preferably 30min; 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. When the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15:1 (mL / g), the ultrasonic extraction temperature is 35°C, the ultrasonic extraction time is 30min, and the ultrasonic power is 360W, 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). It can be seen from this that the method provided in this application is a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from Salvia miltiorrhiza medicinal materials, which can effectively improve the extraction rate, reduce the amount of organic solvent used in the extraction process, and make the extraction operation simpler. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solution of the present application, the drawings required for use in the embodiments are briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

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

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

[0022] Figure 3The flowchart is a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to Example 3 of the present application;

[0023] Figure 4 It is a flow chart of a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to Example 4 of the present application;

[0024] Figure 5 It is a flow chart of a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to Example 5 of the present application;

[0025] Figure 6 It is a flow chart of a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA from salvia miltiorrhiza medicinal materials according to Example 6 of the present application; DETAILED DESCRIPTION

[0026] Example 1

[0027] like Figure 1 As shown, 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, comprising the following steps:

[0028] Step S11, providing a salvia miltiorrhiza raw material, crushing it to obtain salvia miltiorrhiza powder;

[0029] Specifically, the salvia miltiorrhiza medicinal material is dried, crushed by a pulverizer, sieved, and the salvia miltiorrhiza powder under the sieve is obtained.

[0030] Step S12, providing an extraction solvent, which is a mixture of biological source solvents in a certain proportion;

[0031] According to the method described in the Chinese Pharmacopoeia, the extraction methods of tanshinones and salvianolic acid mostly use organic reagents for extraction, such as methanol, 80% methanol. In the present application, a composite solvent composed of at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formal, ethyl lactate, and γ-valerolactone is mixed in a certain proportion, and stirred evenly by manual or magnetic force to obtain an extraction solvent.

[0032] Step S13, mixing the extraction solvent and the Salvia miltiorrhiza powder in a mass ratio of (5-45):1, and ultrasonically extracting at 120-600W to obtain an extracted mixture; the temperature of the ultrasonic extraction is 25-65°C, and the time of the ultrasonic extraction is 5-60min;

[0033] Ultrasonic waves utilize the strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, crushing and stirring effects produced by ultrasonic radiation pressure to increase the frequency and speed of molecular movement of substances and increase the penetration of solvents, thereby accelerating the target ingredients into the solvent and promoting the extraction process.

[0034] The present application is implemented in step three, and the extraction solvent obtained in the above step two and the salvia miltiorrhiza powder obtained in the above step one are mixed according to a certain mass ratio, i.e., liquid-solid ratio, and extracted under ultrasonic conditions. Liquid-solid ratio, extraction temperature, extraction time, and ultrasonic power are important factors affecting the extraction rate. In the method provided in the embodiment of the present application, the liquid-solid ratio is limited to (5-45): 1, the ultrasonic extraction temperature is limited to 25-65 ° C, the ultrasonic extraction time is limited to 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 extracted mixture, taking the supernatant to obtain a salvia miltiorrhiza extract;

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

[0037] The specific implementation methods 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 found in the following examples.

[0038] Example 2

[0039] See also Figure 2 , Example 2 of the present application shows a possible implementation of the method provided by the present application, the extractant solvent of Example 2 includes at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formal, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents, and then the obtained extraction solvent is used to perform ultrasonic extraction on the salvia miltiorrhiza powder, specifically:

[0040] Step S21, providing a salvia miltiorrhiza raw material, pre-treating it, and obtaining 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 formal, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents;

[0042] Step S23, taking 5 identical centrifuge tubes, adding an equal amount of Danshen powder to each centrifuge tube, and then adding the extraction solvent of step S22 to the corresponding centrifuge tube at a liquid-to-solid ratio of 15:1;

[0043] Step S24, fixing the centrifuge tube obtained in step S23 in an ultrasonic cleaning apparatus, and performing ultrasonic extraction for 30 minutes at room temperature to obtain an extracted mixture;

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

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

[0046] Step S26, using high performance liquid chromatography to quantitatively determine the contents of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA in the salvia miltiorrhiza extract of step S25, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA;

[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] As shown in Table 1, in Example 2, when pure water, ethylene glycol, and levulinic acid were used as extraction solvents, the extraction rates of salvianolic acid B, tanshinone I, and cryptotanshinone were relatively high. When glycerol formal was used as the extraction solvent, the extraction rate of tanshinone IIA was the highest.

[0050] Ethylene glycol, levulinic acid, and glycerol formal were used as extraction solvents and compounded in any proportion for extraction. The extraction rate results were summarized and compared, as shown in Table 2:

[0051] Table 2

[0052] Glycerol formal / levulinic acid (57.8 / 42.2, v / v) was screened out as the extraction solvent, and the extraction rates of tanshinone B, tanshinone I, cryptotanshinone, and tanshinone IIA were the highest.

[0053] Example 3

[0054] See also Figure 3 , Example 3 of the present application shows another possible implementation of the method provided by the present application based on the steps described in the aforementioned Example 2. The essential difference from the aforementioned example is that in Example 3, after the salvia miltiorrhiza powder and the extraction solvent are mixed at different liquid-to-solid ratios, ultrasonic extraction is performed under the same conditions; specifically:

[0055] Step S31, providing a salvia miltiorrhiza raw material, pre-treating it, and obtaining salvia miltiorrhiza powder;

[0056] Step S32, providing an extraction solvent; the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v);

[0057] Step S33, take 5 identical centrifuge tubes, add an equal amount of Danshen powder to each centrifuge tube, and then add the extraction solvent of step S32 to the corresponding 5 centrifuge tubes according to the liquid-to-solid ratio of 5:1, 15:1, 25:1, 35:1 and 45:1 respectively;

[0058] Step S34, fixing the centrifuge tube obtained in step S33 in an ultrasonic cleaning apparatus, and ultrasonically extracting for 30 minutes at room temperature to obtain five extracted mixtures;

[0059] Step S35, centrifuging the five extracted mixtures obtained in step S34, taking the supernatant to obtain five extracts;

[0060] Step S36, using high performance liquid chromatography to quantitatively determine the contents of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA in the salvia miltiorrhiza extract of step S35, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA;

[0061] The extraction rate results of Example 3 are summarized and compared, as shown in Table 3:

[0062] Table 3 Extraction rate at different liquid-solid ratios

[0063] 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 preferred liquid-solid ratio of 15:1 is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA.

[0064] Example 4

[0065] See also Figure 4 , Example 4 of the present application shows another possible implementation of the method provided by the present application based on the steps described in the aforementioned Examples 2 and 3. The essential difference from the aforementioned examples is that in Example 4, after the Danshen powder is mixed with the extraction solvent, ultrasonic extraction is performed at different extraction times with other conditions being the same; specifically:

[0066] Step S41, providing a salvia miltiorrhiza raw material, pre-treating it, and obtaining salvia miltiorrhiza powder;

[0067] Step S42, providing an extraction solvent; the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v);

[0068] Step S43, taking 5 identical centrifuge tubes, adding an equal amount of Danshen powder to each centrifuge tube, and adding the extraction solvent of step S42 to the corresponding 5 centrifuge tubes at a liquid-to-solid ratio of 15:1;

[0069] Step S44, fixing the centrifuge tube obtained in step S43 in an ultrasonic cleaning instrument, performing ultrasonic extraction for 5 min, 15 min, 30 min, 45 min, and 60 min at room temperature with an ultrasonic power of 300 W, to obtain five extracted mixtures;

[0070] Step S45, centrifuging the five extracted mixtures obtained in step S44, taking the supernatant to obtain five extracts;

[0071] Step S46, using high performance liquid chromatography to quantitatively determine the contents of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA in the salvia miltiorrhiza extract of step S45, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA;

[0072] The extraction rate results of Example 4 are summarized and compared, as shown in Table 4:

[0073] Table 4 Extraction rate at different extraction times

[0074] 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 by the present application, the preferred extraction time is 30 min, which is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA.

[0075] Example 5

[0076] See also Figure 5 , Example 5 of the present application shows another possible implementation of the method provided by the present application based on the steps described in the aforementioned Examples 2 to 4. The essential difference from the aforementioned examples is that in Example 5, after the Danshen powder is mixed with the extraction solvent, ultrasonic extraction is performed at different extraction temperatures under the same other conditions; specifically:

[0077] Step S51, providing a salvia miltiorrhiza raw material, pre-treating it, and obtaining salvia miltiorrhiza powder;

[0078] Step S52, providing an extraction solvent; the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v);

[0079] Step S53, taking 5 identical centrifuge tubes, adding an equal amount of Danshen powder to each centrifuge tube, and adding the extraction solvent of step S52 to the corresponding 5 centrifuge tubes at a liquid-to-solid ratio of 15:1;

[0080] Step S54, fixing the centrifuge tube obtained in step S53 in an ultrasonic cleaning apparatus, and ultrasonically extracting for 30 min at 25° C., 35° C., 45° C., 55° C., and 65° C., respectively, to obtain five extracted mixtures;

[0081] Step S55, centrifuging the five extracted mixtures obtained in step S54, taking the supernatant to obtain five extracts;

[0082] Step S56, using high performance liquid chromatography to quantitatively determine the contents of salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA in the salvia miltiorrhiza extract of step S55, and calculating the extraction rates of salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA;

[0083] The extraction rate results of Example 5 are summarized and compared, as shown in Table 5:

[0084] Table 5 Extraction rate at different temperatures

[0085] As shown in Table 5, in Example 5, when the extraction temperature is 35°C, 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 in the present application, the preferred extraction temperature is 35°C, which is more conducive to improving the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA.

[0086] Example 6

[0087] See also Figure 6 , Example 6 of the present application shows another possible implementation of the method provided by the present application based on the steps described in the aforementioned Examples 2 to 5. The essential difference from the aforementioned examples is that in Example 6, after the Danshen powder is mixed with the extraction solvent, ultrasonic extraction is performed at different ultrasonic powers under the same other conditions; specifically:

[0088] Step S61, providing a salvia miltiorrhiza raw material, pre-treating it, and obtaining salvia miltiorrhiza powder;

[0089] Step S62, providing an extraction solvent; the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v);

[0090] Step S63, taking 5 identical centrifuge tubes, adding an equal amount of Danshen powder to each centrifuge tube, and adding the extraction solvent of step S62 to the corresponding 5 centrifuge tubes at a liquid-to-solid ratio of 15:1;

[0091] Step S64, fixing the centrifuge tube obtained in step S63 in an ultrasonic cleaning instrument, and ultrasonically extracting for 30 minutes at room temperature at ultrasonic powers of 120 W, 240 W, 360 W, 480 W, and 600 W, to obtain five extracted mixtures;

[0092] Step S65, centrifuging the five extracted mixtures obtained in step S64, taking the supernatant to obtain five extracts;

[0093] Step S66, using high performance liquid chromatography to quantitatively determine the contents of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA in the salvia miltiorrhiza extract of step S65, and calculating the extraction rates of salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA;

[0094] The extraction rate results of Example 6 are summarized and compared, as shown in Table 6:

[0095] Table 6 Extraction rate at different ultrasonic powers

[0096] As shown in Table 6, in Example 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 preferred ultrasonic power is 360 W, which is more conducive to improving the extraction rates of salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA.

[0097] The results showed that when the extraction solvent was glycerol formal / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio was 15:1, the ultrasonic extraction temperature was 35°C, the ultrasonic extraction time was 30 min, and the ultrasonic power was 360 W, it was the best condition for extracting salvianolic acid, tanshinone I, tanshinone, and tanshinone IIA. Compared with the extraction methods of salvianolic acid and tanshinone in the Chinese Pharmacopoeia, as shown in Table 7:

[0098] Table 7 Comparison of extraction methods a: Glycerol formal / levulinic acid (57.8 / 42.2, v / v) b: Extraction method of salvianolic acids in the Danshen standard of the 2020 edition of the Chinese Pharmacopoeia c: Extraction method of tanshinones in the Danshen standard of the 2020 edition of the Chinese Pharmacopoeia

[0099] It can be seen from this that the method provided in the present application for extracting salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from salvia miltiorrhiza can significantly improve the extraction rate.

[0100] 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, using pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formal, ethyl lactate, and γ-valerolactone as extraction solvents, ultrasonically extracting salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from salvia miltiorrhiza powder, the liquid-solid ratio is in the range of (5-45): 1, preferably 15: 1, the extraction solvent is in the range of glycerol formal and levulinic acid composed of a composite solvent, preferably glycerol formal / levulinic acid (57.8 / 42.2, v / v). The ultrasonic extraction power is in the range of 120-600W, preferably 360W. The ultrasonic extraction temperature is in the range of 25-65°C, preferably 35°C. The ultrasonic extraction time is in the range of 5-60min, preferably 30min. The present application embodiment provides a method for extracting salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from salvia miltiorrhiza. When the extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v), the liquid-solid ratio is 15:1, the ultrasonic extraction temperature is 35°C, the ultrasonic extraction time is 30min, and the ultrasonic power is 360W, 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). It can be seen from this that the use of the present application to provide a synchronous green extraction method for extracting salvianolic acid B, tanshinone I, cryptotanshinone, and tanshinone IIA from salvia miltiorrhiza medicinal materials can effectively improve the extraction rate, reduce the amount of organic solvent used in the extraction process, and the extraction operation is simpler.

[0101] The above-described embodiments of the present invention do not limit the protection scope of the present invention.

Claims

1. A synchronous green extraction method for salvianolic acid B, tanshinone I, cryptotanshinone and tanshinone IIA in salvia miltiorrhiza, characterized in that Proceed as follows: Step 1, providing a salvia miltiorrhiza raw material, crushing it to obtain salvia miltiorrhiza powder; Step 2: providing an extraction solvent; the solvent is mixed with biological source solvents in a certain proportion; Step 3, mixing the extraction solvent and the Salvia miltiorrhiza powder in a mass ratio of (5-45):1, and ultrasonically extracting at 120-600W to obtain an extracted mixture; the temperature of the ultrasonic extraction is 25-65°C, and the time of the ultrasonic extraction is 5-60min; Step 4: Centrifuge the extracted mixture, take the supernatant, and obtain the salvia miltiorrhiza extract.

2. The method according to claim 1, characterized in that The extraction solvent includes at least one of pure water, glycerol carbonate, ethylene glycol, levulinic acid, glycerol formal, ethyl lactate, γ-valerolactone and a composite solvent composed of the above solvents.

3. The method according to claim 1 or 2, characterized in that: The extraction solvent is a composite solvent composed of glycerol formal and levulinic acid.

4. The method according to claim 3, characterized in that: The extraction solvent is glycerol formal / levulinic acid (57.8 / 42.2, v / v).

5. The method according to claim 1, characterized in that The extraction solvent and the Salvia miltiorrhiza powder were mixed in a ratio of 15:1 (mL / g).

6. The method according to claim 1, characterized in that The temperature of the ultrasonic extraction is 35°C.

7. The method according to claim 1, characterized in that The ultrasonic extraction time is 30 min.

8. The method according to claim 1, characterized in that The ultrasonic power is 360W.

9. The method according to claim 3, characterized in that: The extraction solvent and salvia miltiorrhiza powder are mixed in a ratio of 15:1 (mL / g), and ultrasonic extraction is performed; the ultrasonic power is 360 W; the ultrasonic extraction time is 30 min, wherein the extractant is glycerol formal / levulinic acid (57.8 / 42.2, v / v).

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