Extraction method of heat-sensitive component in traditional Chinese medicine

Abstract

The extraction method of heat-sensitive components in traditional Chinese medicine in the application comprises the following steps: 1) decocting traditional Chinese medicine containing heat-sensitive components to obtain decocted liquid; 2) storing the decocted liquid; 3) filtering and concentrating to obtain concentrated liquid containing heat-sensitive components; and adding β-cyclodextrin during the extraction of heat-sensitive components in traditional Chinese medicine. The extraction method of heat-sensitive components in traditional Chinese medicine provided by the application can reduce the content attenuation of heat-sensitive components in traditional Chinese medicine caused by the concentration process, storage process and cooling process, improve the transfer efficiency of heat-sensitive components in traditional Chinese medicine, and especially improve the transfer efficiency of curzerene in curcuma.

Description

Technical Field

[0001] The present application relates to the technical field of extraction of effective components of traditional Chinese medicine, and in particular to a method for extracting heat-sensitive components in traditional Chinese medicine. Background Art

[0002] Curcuma zedoaria is used to treat a wide range of conditions and possesses numerous medicinal benefits and benefits, including promoting blood circulation and relieving pain, promoting qi and relieving depression, clearing the heart and cooling blood, and promoting bile secretion and alleviating jaundice. Curcuma zedoaria possesses pungent and bitter properties and a cold nature, acting on the liver, gallbladder, and heart meridians. In Traditional Chinese Medicine, it is used to treat a variety of conditions, including chest and flank pain caused by qi stagnation and blood stasis, coma due to febrile illness, epilepsy, phlegm retention, hematemesis, epistaxis, hematuria, hematuria, as well as jaundice due to damp-heat in the liver and gallbladder, and cholelithiasis.

[0003] Curcumenol, contained in Curcuma formula granules, is an important medicinal ingredient. Research advances indicate that curcumenol possesses antithrombotic, platelet aggregation inhibitory, antitumor, anti-inflammatory, analgesic, and antioxidant properties. Furthermore, curcumenol serves as a potential Q-Marker (quality marker) in Curcuma zedoaria, and together with other chemical components such as curcumol, curcumadione, germacrone, β-elemene, curcumone, curcumadiol, and curcumin, exerts its pharmacological effects through multi-target and multi-pathway interactions. In clinical practice, curcumenol has the efficacy of promoting blood circulation and removing blood stasis, and is commonly used to treat symptoms such as amenorrhea due to blood stasis and abdominal distension caused by food stagnation. It is also one of the main active ingredients in Curcuma zedoaria with lipid-lowering, antioxidant, and anti-inflammatory properties. Curcumenol is also considered a highly effective CYP3A4 inhibitor, exhibiting neuroprotective, anti-inflammatory, anti-tumor, and hepatoprotective activities. In terms of pharmacological effects, curcuminol can significantly inhibit the production of NO in macrophages stimulated by lipopolysaccharide, showing an anti-inflammatory effect.

[0004] Curcuminol is a heat-sensitive active ingredient. However, the traditional production process for turmeric granules easily leads to a decrease in the curcuminol content in the herbal extract during the production process, making it impossible to guarantee product quality.

[0005] In particular, after decocting the turmeric, the hot medicinal juice enters the decoction liquid storage tank directly. After filtration, some of the juice enters the concentrator for concentration until it is fully concentrated. During the production process, due to the large volume of water in the decoction, it cannot be fully transferred to the concentrator at once. Some of the material needs to be stored in the decoction liquid storage tank until the concentrator has sufficient space before it can enter the concentration process to achieve complete concentration. For medicinal juices containing heat-sensitive ingredients, the content will decrease to varying degrees when kept at high temperatures for a long time, making product quality difficult to control.

[0006] Therefore, it is urgent to develop a turmeric extraction process with high curcuminol content. Summary of the Invention

[0007] In order to solve at least one of the above technical problems, the present application provides a method for extracting heat-sensitive components in traditional Chinese medicine.

[0008] In the first aspect of the present application, the present application provides a method for extracting heat-sensitive components in traditional Chinese medicine, comprising:

[0009] Step 1): decocting the traditional Chinese medicine containing heat-sensitive components to obtain a decoction;

[0010] Step 2): storing the decoction;

[0011] Step 3): Filter and concentrate to obtain a concentrated solution containing heat-sensitive components;

[0012] β-cyclodextrin is added during the extraction of heat-sensitive components in traditional Chinese medicine.

[0013] Through the above technical solution, β-cyclodextrin has an inclusion effect on the heat-sensitive components, which can reduce the attenuation of the heat-sensitive components in traditional Chinese medicine.

[0014] Preferably, the step 1) further comprises cooling the decocted liquid at a cooling rate of 40-100° C. / h.

[0015] Through the above technical solution, the cooling rate is controlled to 40-100℃ / h, which can control the heat-sensitive components in traditional Chinese medicine within the tolerance range of temperature and temperature changes, and reduce the attenuation of the heat-sensitive components of traditional Chinese medicine.

[0016] Preferably, the cooling treatment is to cool the temperature to 60-80°C.

[0017] Preferably, the β-cyclodextrin is added after decocting in step 1) and before cooling and / or after cooling in step 1) and / or after filtering and before concentration in step 3).

[0018] Through the above technical solution, by adjusting the timing of adding β-cyclodextrin, the degradation of heat-sensitive components during temperature changes, storage and concentration processes can be reduced to a greater extent, thereby improving the extraction efficiency of heat-sensitive components.

[0019] Preferably, in step 3), the concentration temperature is 55 to 65° C., and the vacuum degree is -0.06 to -0.08 MPa.

[0020] The above technical solution, combined with specific concentration conditions, can effectively improve the extraction effect of heat-sensitive components in traditional Chinese medicine.

[0021] Preferably, the traditional Chinese medicine is Curcuma zedoaria, and the heat-sensitive component is curcumenol.

[0022] Preferably, in step 1), the decoction is performed 1-3 times, the weight of water added in each decoction is 10-12 times the weight of the Chinese medicine, and the decoction time for each decoction is 1-1.5 hours.

[0023] Preferably, the mass of the added β-cyclodextrin is 3-10% of the traditional Chinese medicine, preferably 5%.

[0024] In a second aspect of the present application, the present application provides the use of β-cyclodextrin in improving the extraction efficiency of heat-sensitive components in traditional Chinese medicine containing heat-sensitive components.

[0025] Preferably, the traditional Chinese medicine is Curcuma zedoaria, and the heat-sensitive component is curcumenol.

[0026] In summary, the present invention includes at least one of the following beneficial technical effects:

[0027] 1. The present invention provides a method for extracting heat-sensitive components in traditional Chinese medicine, which can reduce the content attenuation of heat-sensitive components in traditional Chinese medicine caused by the concentration process, reduce the content attenuation of heat-sensitive components in the storage process, and reduce the content attenuation of heat-sensitive components in the cooling process; 2. The present invention improves the transfer efficiency of heat-sensitive components in traditional Chinese medicine, especially the transfer efficiency of curcuminol in turmeric, by adding β-cyclodextrin during the extraction process and controlling factors such as the cooling rate during the cooling process, the final cooling temperature, the temperature and vacuum degree during concentration, and the timing of adding β-cyclodextrin. DETAILED DESCRIPTION

[0028] The present invention will be further described below in conjunction with specific examples, but the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. In the following examples, if no specific conditions are specified, the conditions according to normal conditions or manufacturer's recommendations are carried out, and the method used, if not otherwise specified, is a conventional method well known in the art, and the consumable materials and reagents used, if not otherwise specified, are commercially available. Unless otherwise indicated, the professional and scientific terms used herein are identical in meaning to those skilled in the art. In addition, any method or material similar or equivalent to the described content can also be applied to the present invention.

[0029] In the first aspect of the present application, the present application provides a method for extracting heat-sensitive components in traditional Chinese medicine, comprising:

[0030] Step 1): decocting the traditional Chinese medicine containing heat-sensitive components to obtain a decoction;

[0031] Step 2): storing the decoction;

[0032] Step 3): Filter and concentrate to obtain a concentrated solution containing heat-sensitive components;

[0033] β-cyclodextrin is added during the extraction of heat-sensitive components in traditional Chinese medicine.

[0034] Preferably, the step 1) further comprises a cooling process of the decocted liquid, and the cooling rate is controlled to be 40-100℃ / h.

[0035] Preferably, the cooling process is cooling to 60-80℃.

[0036] Preferably, the β-cyclodextrin is added before the cooling process after decocting in step 1) and / or added after the cooling process in step 1) and / or added before the concentration after filtering in step 3).

[0037] Preferably, in the step 3), the concentration temperature is 55-65℃, and the vacuum degree is -0.06 to -0.08 MPa.

[0038] Preferably, the traditional Chinese medicine is Curcuma zedoary, and the heat-sensitive component is zedoary alcohol.

[0039] Preferably, in the step 1), the decoction is performed for 1-3 times, and the weight of water added in each decoction is 10-12 times of the weight of the traditional Chinese medicine, and the decoction time of each decoction is 1-1.5h.

[0040] Preferably, the mass of the β-cyclodextrin added is 3-10% of the traditional Chinese medicine, preferably 5%.

[0041] In the second aspect of the present application, the present application provides the use of β-cyclodextrin in improving the extraction efficiency of heat-sensitive components in traditional Chinese medicines containing heat-sensitive components. Specific embodiments

[0043] The content of zedoary alcohol in the Curcuma zedoary decoction pieces used in the examples and comparative examples is 0.07%.

[0044] Example 1

[0045] Take 300 kg of Curcuma zedoary decoction pieces to the extraction tank, and extract for 2 times. The first time, add water with a weight of 10 times of the weight of the traditional Chinese medicine, and decoct at 100℃ for 1.5 hours. The second time, add water with a weight of 8 times of the weight of the traditional Chinese medicine, and decoct at 100℃ for 1 hour. Transfer the decocted liquid to the decocted liquid cooling device, add 15 kg of β-cyclodextrin, and stir uniformly. After 0.5h, cool to 60℃, and the cooling rate is 80℃ / h. Transfer to the decocted liquid storage tank, and store at the constant temperature of the cooling endpoint temperature for 24h. Filter, concentrate, and control the concentration temperature to be 55℃, and the vacuum degree to be -0.08 MPa. Concentrate to a specific gravity of 1.09 to obtain a concentrate containing zedoary alcohol.

[0046] Example 2-3

[0047] Example 2

[0048] The difference between Example 2 and Example 1 is that after being transferred to the decocted liquid cooling device, it is cooled to 60℃ after 1h, and the cooling rate is 40℃ / h.

[0049] Example 3

[0050] The difference between Example 3 and Example 1 is that the decoction liquid is transferred to a decoction liquid cooling device and cooled to 60° C. after 0.4 h at a cooling rate of 100° C. / h.

[0051] Examples 4-5

[0052] Example 4

[0053] The difference between Example 4 and Example 1 is that the decoction liquid is transferred to the decoction liquid cooling device, the cooling rate remains unchanged, and the decoction liquid is cooled to 70°C.

[0054] Example 5

[0055] The difference between Example 5 and Example 1 is that the decoction liquid is transferred to the decoction liquid cooling device, the cooling rate remains unchanged, and the decoction liquid is cooled to 80°C.

[0056] Example 6

[0057] The difference between Example 6 and Example 1 is that the concentration temperature is 65° C. and the vacuum degree is -0.06 MPa.

[0058] Examples 7-8

[0059] Example 7

[0060] 300 kg of turmeric slices were put into an extraction tank and extracted with water twice. The first time, 10 times the weight of the medicinal material was added with water, and the mixture was decocted at 100° C. for 1.5 hours. The second time, 8 times the weight of the medicinal material was added with water, and the mixture was decocted at 100° C. for 1 hour. The decoction was transferred to a decoction cooling device, cooled to 60° C. after 0.5 hours, with a cooling rate of 80° C. / h, 15 kg of β-cyclodextrin was added, and the mixture was transferred to a decoction storage tank and stored at a constant temperature at the cooling end temperature for 24 hours. The mixture was filtered and concentrated at a concentration temperature of 55° C. and a vacuum degree of -0.08 MPa. The mixture was concentrated to a specific gravity of 1.09 to obtain a concentrate containing curcuminol.

[0061] Example 8

[0062] 300 kg of turmeric slices were put into an extraction tank and extracted with water twice. The first time, 10 times the weight of the medicinal materials was added with water, and the mixture was decocted at 100° C. for 1.5 hours. The second time, 8 times the weight of the medicinal materials was added with water, and the mixture was decocted at 100° C. for 1 hour. The decoction was transferred to a decoction cooling device, cooled to 60° C. after 0.5 hours, with a cooling rate of 80° C. / h, transferred to a decoction storage tank, and stored at a constant temperature at the cooling end temperature for 24 hours. The mixture was filtered, 15 kg of β-cyclodextrin was added, and the mixture was concentrated at a concentration temperature of 55° C. and a vacuum degree of -0.08 MPa. The mixture was concentrated to a specific gravity of 1.09 to obtain a concentrate containing curcuminol.

[0063] Example 9

[0064] 300 kg of turmeric slices were put into an extraction tank and extracted with water twice. The first time, 10 times the weight of the medicinal material was added with water and decocted at 100° C. for 1.5 hours. The second time, 8 times the weight of the medicinal material was added with water and decocted at 100° C. for 1 hour. 15 kg of β-cyclodextrin was added and the decoction was transferred to a decoction storage tank and stored at a constant temperature for 24 hours. The decoction was filtered and concentrated at a concentration temperature of 55° C. and a vacuum degree of -0.08 MPa. The decoction was concentrated to a specific gravity of 1.09 to obtain a concentrate containing curcuminol.

[0065] Example 10

[0066] 300 kg of turmeric slices were put into an extraction tank and extracted with water twice. The first time, 10 times the weight of the medicinal materials was added with water, and the mixture was decocted at 100° C. for 1.5 hours. The second time, 8 times the weight of the medicinal materials was added with water, and the mixture was decocted at 100° C. for 1 hour. 11.25 kg of β-cyclodextrin was added, and the decoction was transferred to a decoction cooling device. After 0.5 hours, the decoction was cooled to 60° C. at a cooling rate of 80° C. / h. The decoction was transferred to a decoction storage tank and stored at a constant temperature at the cooling end temperature for 24 hours. The decoction was filtered, 3.75 kg of β-cyclodextrin was added, and the mixture was concentrated at a concentration temperature of 55° C. and a vacuum degree of -0.08 MPa. The decoction was concentrated to a specific gravity of 1.09 to obtain a concentrate containing curcuminol.

[0067] Comparative Example 1

[0068] The only difference between Comparative Example 1 and Example 1 is that β-cyclodextrin is not added.

[0069] Comparative Example 2

[0070] Take 300 kg of Curcuma aromatica slices into an extraction tank and extract them with water twice. The first time, add 12 times the weight of the medicinal materials with water and boil them at 100°C for 1.5 hours. The second time, add 10 times the weight of the medicinal materials with water and boil them at 100°C for 1 hour. Transfer the decoction to a decoction storage tank and store it at a constant temperature for 24 hours. Filter and concentrate it at a concentration temperature of 55°C and a vacuum degree of -0.08 MPa. Concentrate it to a specific gravity of 1.09 to obtain a concentrate.

[0071] Comparative Example 3

[0072] Take 300 kg of Curcuma aromatica slices into an extraction tank, add water to extract twice, add 12 times the weight of the medicinal material water for the first time, and decoct at 100°C for 1.5 hours; add 10 times the weight of the medicinal material water for the second time, and decoct at 100°C for 1 hour. Transfer the decoction to a decoction liquid storage tank, naturally cool to room temperature, and store for 24 hours. Filter and concentrate. The concentration temperature is 55°C and the vacuum degree is -0.08Mpa. Concentrate to a specific gravity of 1.09 to obtain a concentrate.

[0073] Experimental testing

[0074] The curcumenol content in turmeric slices and concentrates containing curcumenol was determined according to standard chromatographic conditions and system suitability tests using octadecylsilane bonded silica gel as the filler; acetonitrile-0.1% phosphoric acid solution (56:44) as the mobile phase; a detection wavelength of 262 nm, and isocratic elution. The number of theoretical plates calculated based on the curcumenol peak should be no less than 5000.

[0075] Preparation of test solution: Take an appropriate amount of this product, about 4.0g, accurately weigh, place in a stoppered conical flask, accurately add 10ml of 75% methanol, weigh the weight, ultrasonically treat (power 1130W, frequency 37kHz) for 15 minutes, let cool, weigh again, make up the lost weight with 75% methanol, shake well, filter, and take the filtrate.

[0076] Preparation of reference solution: Take an appropriate amount of curcuminol reference substance, accurately weigh it, and add 75% methanol to make a solution containing 13 μg of curcuminol per 1 ml.

[0077] Determination method: Accurately aspirate 20 μl of reference solution and test solution respectively, inject into liquid chromatograph, and determine.

[0078] Content transfer rate (%) = (mass of the concentrate containing curcuminol × content of curcuminol in the concentrate containing curcuminol) ÷ (mass of turmeric slices × content of curcuminol in turmeric slices)

[0079] The contents of curcuminol in the turmeric slices and the concentrate containing curcuminol in the examples and comparative examples were respectively detected, and the content transfer rates were calculated. The results are shown in Table 1.

[0080] Table 1 Content transfer rate of curcuminol in Examples and Comparative Examples

[0081] Test items Content transfer rate (%) Example 1 27.5 Example 2 20.3 Example 3 27.0 Example 4 15.7 Example 5 11.3 Example 6 9.8 Example 7 26.3 Example 8 27.0 Example 9 17.5 Example 10 26.5 Comparative Example 1 11.5 Comparative Example 2 6.1 Comparative Example 3 6.8

[0082] From the test results in Table 1, it can be seen that, compared with Example 1, Examples 2 and 3, adjusting the cooling rate has a certain effect on the extraction efficiency of the heat-sensitive component curcuminol in Curcuma. This may be because curcuminol has a limited tolerance to temperature changes, and a cooling rate that is too fast or too slow will accelerate the degradation of curcuminol.

[0083] Comparison of Examples 4 and 5 with Example 1 shows that the final cooling temperature affects the extraction efficiency of curcuminol, a heat-sensitive component in Curcuma.

[0084] Comparison of Example 6 with Example 1 shows that the concentration temperature and vacuum degree during concentration have a significant effect on the extraction efficiency of curcuminol, a heat-sensitive component in Curcuma.

[0085] Comparison of Examples 7 and 8 with Example 1 shows that the timing of adding β-cyclodextrin affects the extraction efficiency of curcuminol from the concentrate. This may be because β-cyclodextrin has an inclusion complexing effect on curcuminol, which can reduce the degradation of curcuminol during temperature changes, storage, and concentration.

[0086] Comparison of Example 9 with Example 1 shows that when there is no cooling step, the extraction efficiency of the heat-sensitive component curcumenol in Curcuma is low.

[0087] Comparison of Example 10 with Example 1 shows that adding β-cyclodextrin before cooling and before concentration respectively cannot improve the extraction effect of curcuminol in traditional Chinese medicine.

[0088] Comparison of Comparative Examples 1-3 with the Example shows that without adding β-cyclodextrin, the extraction efficiency of the heat-sensitive component curcumenol in Curcuma is low. Without adding β-cyclodextrin and without a cooling process, directly storing at a constant temperature or naturally cooling to room temperature for storage, the extraction efficiency of the heat-sensitive component curcumenol in Curcuma is even lower.

[0089] The above are all preferred embodiments of the present application, and are not intended to limit the scope of protection of the present application. Therefore, any equivalent changes made based on the structure, shape, and principle of the present application should be included in the scope of protection of the present application.

Claims

1. A method for extracting heat-sensitive components in traditional Chinese medicine, characterized in that: include: Step 1): decocting a traditional Chinese medicine containing a heat-sensitive component to obtain a decoction; Step 2): storing the decoction; Step 3): filtering and concentrating to obtain a concentrated solution containing the heat-sensitive component; adding β-cyclodextrin during the extraction process of the heat-sensitive component in the traditional Chinese medicine; The step 1) further comprises cooling the decoction liquid, controlling the cooling rate to be 40-100°C / h; The cooling treatment is to cool the temperature to 60°C; The β-cyclodextrin is added after the decoction in step 1) and before the cooling treatment and / or after the cooling treatment in step 1) and / or after the filtration and before the concentration in step 3); In step 3), the concentration temperature is 55°C and the vacuum degree is -0.08 MPa; The traditional Chinese medicine is Curcuma zedoaria, and the heat-sensitive component is curcumenol; The mass of the added beta-cyclodextrin is 3-10% of the traditional Chinese medicine.

2. The method for extracting heat-sensitive components in traditional Chinese medicine according to claim 1, wherein In the step 1), the medicine is decocted for 1-3 times, the weight of water added in each decoction is 10-12 times the weight of the Chinese medicine, and the decoction time for each decoction is 1-1.5 hours.