Method for increasing content of agarotetrol in agilawood medicinal material

Abstract

The invention relates to the technical field of traditional Chinese medicines, and particularly provides a method for increasing the content of agilawood tetrol in agilawood medicinal materials. Comprising the following steps: chopping an agilawood raw medicinal material into small blocks; spreading the small pieces of agilawood medicinal materials on a stainless steel tray from top to bottom, putting the stainless steel tray into a pulsating vacuum steam sterilizer, and closing a cabinet door; starting a pulsating vacuum steam sterilizer, draining water and starting steam for preheating before the sterilizer is used so as to prevent condensed water from splashing on the medicinal materials, and setting the treatment temperature to be 105-121 DEG C, the treatment time to be 20-30 minutes and the drying time to be 5-10 minutes; and taking out the stainless steel tray after the treatment is finished, cooling to room temperature under the room temperature condition, and collecting the material. The method disclosed by the invention is simple and quick to operate, time-saving and labor-saving, the content of the agilawood tetrol in the agilawood medicinal material can be remarkably increased only by adopting a physical heating mode, meanwhile, other indexes specified by the existing pharmacopoeia can meet the requirements, the problem of low content of the agilawood medicinal material can be effectively solved, and a technical support is provided for resource utilization of the agilawood medicinal material and development of a traditional Chinese medicine preparation.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicines, and in particular to a method for increasing the content of agarwood tetraol in agarwood medicinal materials. Background Art

[0002] Agarwood is a resin-containing wood of Aquilaria sinensis (Lour.) Gilg, a plant of the Thymelaeaceae family. It is mainly distributed in Guangdong, Guangxi, Hainan, Yunnan, Fujian and Taiwan in my country. It tastes spicy and bitter, is slightly warm in nature, and has the effects of promoting qi and relieving pain, warming the middle and stopping vomiting, and relieving asthma. It is mainly used for chest and abdominal distension and pain, stomach cold vomiting and hiccups, kidney deficiency, qi reversal and asthma. Modern pharmacological studies have shown that agarwood has multiple biological activities such as antibacterial, hypoglycemic, anti-inflammatory, and anti-tumor, and has certain pharmacological effects on the central nervous system, respiratory system, digestive system, etc., showing the pharmacological effects of sedation and hypnosis, cough and asthma relief, and intestinal spasmolysis. Therefore, agarwood also has good medicinal value.

[0003] Agarwood contains complex chemical components, including monoterpenes, sesquiterpenes, diterpenes, triterpenes, sterols, flavonoids, chromones, phenolic acids and aliphatic compounds, which give agarwood its unique fragrance and medicinal value. Agarwood tetraol is a chromone compound. The 2015 edition of the Chinese Pharmacopoeia included agarwood tetraol content in the pharmacopoeia for the first time as one of the key indicators for quality control of agarwood. Many agarwood materials on the market are substandard due to insufficient agarwood tetraol content, which is not conducive to the resource utilization of agarwood, a precious Chinese medicinal material.

[0004] In view of this, how to increase the content of agarwood tetraol in agarwood medicinal materials has become a technical problem that needs to be solved urgently. Summary of the invention

[0005] In view of this, the present invention proposes a method for increasing the content of agarwood tetraol in agarwood medicinal materials. This method can significantly increase the content of agarwood tetraol in agarwood medicinal materials, thereby solving the problem that the content of agarwood tetraol in agarwood medicinal materials is low, which is not conducive to the resource utilization of agarwood medicinal materials.

[0006] The technical solution of the present invention is achieved as follows: The present invention provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, comprising the following steps:

[0007] Step 1: Chop the agarwood into small pieces;

[0008] Step 2: Spread the small pieces of agarwood obtained in step 1 on a stainless steel tray with a thickness of ≤30 mm, and place it in a pulsating vacuum steam sterilizer;

[0009] Step 3: Start pulsating vacuum steam sterilization, the processing temperature is 105-121°C, the processing time is 20-30 minutes, and the drying time is 5-10 minutes;

[0010] Step 4: After processing, take out the stainless steel tray and cool it to room temperature before collecting the material.

[0011] In some embodiments, the small piece has a length of 0.3-5.0 cm, a width of 0.2-3.0 cm, and a thickness of 0.1-0.5 cm.

[0012] In some embodiments, in step 2, the thickness of the paving disc is ≤ 20 mm.

[0013] In some embodiments, in step 2, the closest distance between the agarwood medicinal material and the edge of the tray is no less than 1 cm.

[0014] In some embodiments, the agarwood medicinal material is subjected to a surface impurity removal treatment, and the impurity removal treatment method includes removing dead white wood and other impurities on the surface.

[0015] In some embodiments, in step three, the treatment temperature is 121° C., the treatment time is 30 min, and the drying time is 5 min.

[0016] In a second aspect, the present invention further provides an agarwood medicinal material, which is obtained by processing using the method described in any one of claims 1 to 6.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] The processing method of the present invention has fewer steps, is simple and fast to operate, has low energy consumption cost, and can significantly improve the quality of agarwood, a precious and fine medicinal material, at a relatively low cost. The present invention can improve the content of agarwood medicinal materials by only using relatively simple physical operations. After wet heat treatment, other pharmacopoeia-specified indicators such as characteristic spectra, extracts, and thin layer identification all meet the requirements of the current edition of the "Chinese Pharmacopoeia", and the properties of the medicinal materials are not changed. The problem that the content of agarwood medicinal materials is low and does not meet the quality requirements can be effectively solved, and technical support is provided for the full utilization of agarwood medicinal material resources and the development of related preparations. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0020] Figure 1 This is the characteristic spectrum of the agarwood medicinal material of the untreated group of the present invention;

[0021] Figure 2 This is the characteristic spectrum of the medicinal material after being processed in Example 1 of the present invention;

[0022] Figure 3 This is the characteristic spectrum of the medicinal material after being processed in Example 2 of the present invention;

[0023] Figure 4 This is the characteristic spectrum of the medicinal material after being processed in Example 3 of the present invention;

[0024] Figure 5 This is the characteristic spectrum of the medicinal material after being treated in Comparative Example 1 of the present invention;

[0025] Figure 6 This is the characteristic spectrum of the medicinal material after being treated in Comparative Example 2 of the present invention;

[0026] Figure 7 This is the characteristic spectrum of the medicinal material after being treated in Comparative Example 3 of the present invention;

[0027] Figure 8 This is the characteristic spectrum of the medicinal materials after the first batch of treatment in Example 4 of the present invention;

[0028] Fig. 9 This is the characteristic spectrum of the medicinal materials after the second batch of processing in Example 4 of the present invention;

[0029] Fig.10 This is the characteristic spectrum of the medicinal materials after the third batch of treatment in Example 4 of the present invention;

[0030] Fig.11 The thin layer identification chromatograms of the medicinal materials of Examples 1-3 of the present invention and the untreated group;

[0031] Fig.12 The chromatograms are thin layer identification chromatograms of different batches of medicinal materials and untreated group in Example 4 of the present invention. DETAILED DESCRIPTION

[0032] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the embodiments of the present invention belong. If the definitions set forth in this section are contrary to or otherwise inconsistent with the definitions set forth in the patents, patent applications, published patent applications, and other publications incorporated herein by reference, the definitions listed in this section take precedence over the definitions incorporated herein by reference.

[0034] Unless otherwise specified, the methods used in the following examples are all conventional methods. Unless otherwise specified, the materials, reagents and instruments used are all conventional materials, reagents and instruments in the art, and can be obtained by those skilled in the art through commercial channels.

[0035] When an amount, concentration or other value or parameter is expressed as a range, a preferred range or a range defined by a series of upper preferred values ​​and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value with any range lower limit or preferred value, regardless of whether the range is disclosed separately. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted as including the range "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5", etc. When a numerical range is described herein, unless otherwise stated, the range is intended to include its end values ​​and all integers and fractions within the range. In the present specification and claims, range definitions can be combined and / or interchanged, and if not otherwise stated, these ranges include all subranges contained therein.

[0036] The same batch of agarwood medicinal materials were used for treatment verification in the following examples and comparative examples, and the original medicinal materials before treatment were tested for agarwood medicinal material content, characteristic spectrum, extracts and other indicators according to the current edition of the "Chinese Pharmacopoeia" to obtain the untreated group data, among which the thin layer identification chromatogram is as follows Fig.11 4 and Fig.12 As shown in 4.

[0037] Example 1.

[0038] This embodiment provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0039] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 0.3-2.0cm, a width of 0.2-1.0cm, and a thickness of 0.1-0.2cm;

[0040] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 on a stainless steel tray from top to bottom, with a thickness of ≤10mm, and put them into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0041] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 105°C, the processing time to 20 minutes, and the drying time to 10 minutes.

[0042] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0043] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 1 As shown, the thin layer identification chromatogram is as follows Fig.11 As shown in 1.

[0044] Example 2

[0045] This embodiment provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0046] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 1.0-2.5cm, a width of 0.5-2.5cm, and a thickness of 0.2-0.3cm;

[0047] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 from top to bottom on a stainless steel tray with a thickness of ≤20mm, put it into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0048] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 116°C, the processing time to 30 minutes, and the drying time to 7 minutes.

[0049] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0050] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 2 As shown, the thin layer identification chromatogram is as follows Fig.11 As shown in 2.

[0051] Example 3

[0052] This embodiment provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0053] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 1.5-3.5cm, a width of 1.0-3.0cm, and a thickness of 0.3-0.5cm;

[0054] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 on a stainless steel tray from top to bottom, with a thickness of ≤30mm, and put them into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0055] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 121°C, the processing time to 20 minutes, and the drying time to 5 minutes.

[0056] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0057] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 3 As shown, the thin layer identification chromatogram is as follows Fig.11 As shown in 3.

[0058] Comparative Example 1

[0059] This comparative example provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0060] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 0.3-2.0cm, a width of 0.2-1.0cm, and a thickness of 0.1-0.2cm;

[0061] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 on a stainless steel tray from top to bottom, with a thickness of ≤10mm, and put them into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0062] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 80°C, the processing time to 20 minutes, and the drying time to 10 minutes.

[0063] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0064] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 4 shown.

[0065] Comparative Example 2

[0066] This comparative example provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0067] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 1.0-2.5cm, a width of 0.5-2.5cm, and a thickness of 0.2-0.3cm;

[0068] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 from top to bottom on a stainless steel tray with a thickness of ≤20mm, put it into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0069] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 90°C, the processing time to 30 minutes, and the drying time to 7 minutes.

[0070] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0071] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 5 shown.

[0072] Comparative Example 3

[0073] This comparative example provides a method for increasing the content of agarwood tetraol in agarwood medicinal materials, and the steps are as follows:

[0074] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 1.5-3.5cm, a width of 1.0-3.0cm, and a thickness of 0.3-0.5cm;

[0075] Step 2: Spread the agarwood medicinal materials chopped into small pieces in step 1 on a stainless steel tray from top to bottom, with a thickness of ≤30mm, and put them into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0076] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 150°C, the processing time to 20 minutes, and the drying time to 5 minutes.

[0077] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0078] Step 5: Take the agarwood material treated in step 4 and test the agarwood material content, characteristic spectrum, extract and other indicators according to the current edition of the Chinese Pharmacopoeia. Figure 6 shown.

[0079] The test results of the medicinal materials of the above different embodiments and comparative examples are shown in the following table:

[0080] Test items Untreated group Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Agarwood tetraol content / % 0.152 0.242 0.250 0.260 0.162 0.165 0.144 Feature Spectrum conform to conform to conform to conform to conform to conform to conform to Extract / % 13.6 16.6 17.2 16.7 14.4 14.8 13.8 Thin layer identification conform to conform to conform to conform to conform to conform to conform to Content changes - 59.21％ 64.47％ 71.05％ 6.58％ 8.55％ -5.26％

[0081] It can be seen from the data in the table that compared with the untreated group, the content of agarwood tetraol in the medicinal material after wet heat treatment in Examples 1, 2, and 3 increased by 59.21%, 64.47%, and 71.05%, respectively. The content of Comparative Examples 1 and 2 did not change much compared with the untreated group, and only increased by 6.58% and 8.55%, respectively. The wet heat treatment temperature of Comparative Example 3 was significantly higher than that of each embodiment and Comparative Examples 1 and 2, and the content of agarwood tetraol in the medicinal material was lower than that of the untreated group, which decreased by 5.26% (the content of agarwood tetraol in the medicinal material was calculated based on the dry product). Chromone compounds are a class of compounds with a special skeleton structure, and their derivatives are numerous. Chromone compounds, especially 2-(2-phenylethyl) chromone compounds, are unique compounds of agarwood medicinal materials. Agarwood tetraol, as a type of 2-(2-phenylethyl) chromone compounds, has a relatively simple structure. Under certain conditions, there is the possibility that other chromone compounds are converted into agarwood tetraol. This may be the main reason why wet heat treatment can significantly increase the content of agarwood tetraol in agarwood medicinal materials.

[0082] Among the other test items specified under the agarwood medicinal material item in the current edition of the "Chinese Pharmacopoeia", the characteristic spectra, extracts, and thin layer identifications of the agarwood medicinal materials after treatment in each embodiment and comparative example all meet the requirements of the Pharmacopoeia. Even in terms of alcohol-soluble extracts, compared with the untreated group, the content of alcohol-soluble extracts of the agarwood medicinal materials in each embodiment increased, while the comparative examples did not change much.

[0083] Combining the detection results of various indicators of the above embodiments and comparative examples, it can be seen that the content of agarwood tetraol in the agarwood medicinal material is significantly increased after wet heat treatment. Under the set experimental conditions, the content of agarwood tetraol can be increased by up to 71.05%. At the same time, other detection items specified in the Pharmacopoeia, such as characteristic spectra, extracts, thin layer identification, etc., all meet the requirements of the Pharmacopoeia.

[0084] In order to verify the operability and feasibility of the above results in actual production, the present invention also combines the actual workshop, enlarges the processing batch, and verifies three batches of medicinal materials. The examples are as follows:

[0085] Example 4

[0086] Step 1: Take the original agarwood material, remove the dead white wood and other impurities on the surface, and split it into small pieces with a length of 0.3-4.0cm, a width of 0.2-2.0cm, and a thickness of 0.1-0.4cm;

[0087] Step 2: Spread about 20 kg of the agarwood medicinal materials chopped into small pieces in step 1 on a stainless steel tray from top to bottom, with the thickness of each tray ≤ 20 mm, and put them into the SCM-DJSB pulsating vacuum steam sterilizer, and close the cabinet door;

[0088] Step 3: Turn on the SCM-DJSB pulsating vacuum steam sterilizer. Drain the sterilizer and preheat it with steam before use to avoid condensed water splashing on the medicinal materials. Set the processing temperature to 121°C, the processing time to 30 minutes, and the drying time to 5 minutes.

[0089] Step 4: After the treatment is completed, take out the stainless steel tray, cool it to room temperature and then collect the material;

[0090] Step 5: Take the agarwood materials treated in step 4 and test the agarwood materials content, characteristic spectrum, extracts and other indicators according to the current edition of the Chinese Pharmacopoeia. The thin layer identification chromatograms of the three batches are as follows: Fig.12 As shown in 1, 2, and 3.

[0091] The test results of three batches of medicinal materials for verification experiment in Example 4 are as follows:

[0092] Test items Untreated group First batch of verification Second batch of verification The third batch of verification Agarwood tetraol content / % 0.152 0.263 0.266 0.259 Feature Spectrum conform to conform to conform to conform to Extract / % 13.6 17.4 18.3 16.9 Thin layer identification conform to conform to conform to conform to Content changes - 73.03 75％ 70.39％

[0093] In order to facilitate workshop production operations and improve production efficiency, combined with the preferred wet heat treatment conditions of the previous embodiments, that is, 121°C wet heat treatment for 30 minutes, drying for 5 minutes after treatment, three batches of agarwood medicinal materials were treated. As can be seen from Table 2, the content of agarwood tetraol in the three batches of agarwood medicinal materials in the amplification verification experiment in Example 4 was increased by 73.03%, 75%, and 70.39% respectively compared with the untreated original medicinal materials, with an average increase of 72.81%, and the RSD value was 3.18%. At the same time, the characteristic spectra, extracts, and thin layer identification of the three batches of agarwood medicinal materials after wet heat treatment all met the requirements of the pharmacopoeia.

[0094] The above results show that the technical solution of the present invention is simple and quick to operate, has few steps, is easy to implement, and can significantly increase the content of agarwood tetraol in agarwood medicinal materials only through physical treatment methods. At the same time, other indicators specified in the pharmacopoeia after treatment, such as characteristic spectra, extracts, thin layer identification, etc., can meet the requirements, and it has strong practical value.

[0095] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for increasing the content of agarwood tetraol in agarwood medicinal material, characterized in that: The steps include: Step 1: Chop the agarwood into small pieces; Step 2: Spread the small pieces of agarwood obtained in step 1 on a stainless steel tray with a thickness of ≤30 mm, and place them in a pulsating vacuum steam sterilizer; Step 3: Start pulsating vacuum steam sterilization, the processing temperature is 105-121°C, the processing time is 20-30 minutes, and the drying time is 5-10 minutes; Step 4: After processing, take out the stainless steel tray and cool it to room temperature before collecting the material.

2. The method for increasing the content of agarwood tetraol in agarwood medicinal material according to claim 1, characterized in that: The length of the small piece is 0.3-5.0 cm, the width is 0.2-3.0 cm, and the thickness is 0.1-0.5 cm.

3. The method for increasing the content of agarwood tetraol in agarwood medicinal material according to claim 1, characterized in that: In step 2, the thickness of the plate is ≤20mm.

4. The method for increasing the content of agarwood tetraol in agarwood medicinal material according to claim 1, characterized in that: In step 2, the closest distance between the agarwood material and the edge of the tray is no less than 1 cm.

5. The method for increasing the content of agarwood tetraol in agarwood medicinal material according to claim 1, characterized in that: The agarwood medicinal material undergoes surface impurity removal treatment, which includes removing dead white wood and other impurities on the surface.

6. The method for increasing the content of agarwood tetraol in agarwood medicinal material according to claim 1, characterized in that: In step three, the treatment temperature is 121° C., the treatment time is 30 min, and the drying time is 5 min.

7. An agarwood medicinal material, characterized in that: The agarwood medicinal material is obtained by processing using the method described in any one of claims 1 to 6.

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