CN111664661A - Vacuum drying method without damaging effective components of radix Angelicae sinensis - Google Patents
Vacuum drying method without damaging effective components of radix Angelicae sinensis Download PDFInfo
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- CN111664661A CN111664661A CN202010492194.7A CN202010492194A CN111664661A CN 111664661 A CN111664661 A CN 111664661A CN 202010492194 A CN202010492194 A CN 202010492194A CN 111664661 A CN111664661 A CN 111664661A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/044—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum for drying materials in a batch operation in an enclosure having a plurality of shelves which may be heated
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Abstract
The invention relates to a vacuum drying method without damaging effective components of Chinese angelica, which comprises the following steps: pre-treating, vacuum drying, stopping heating after drying, discharging after vacuum discharge, finishing, sealing and storing. The angelica medicinal material treated by the method effectively ensures that the effective components in the angelica medicinal material are not damaged, the appearance form of the vacuum-dried angelica is better kept and is close to that of a fresh medicinal material, the medicinal material can be dried at a lower temperature in a vacuum state, the drying time is shorter, and the energy is saved. Meanwhile, the method is simple and easy to implement, has strong practicability and is suitable for large-scale production.
Description
Technical Field
The invention relates to a drying method of angelica, in particular to a vacuum drying method without damaging the effective components of the angelica, belonging to the field of processing of traditional Chinese medicinal materials.
Background
With the development of science and technology, the drying and processing modes of traditional Chinese medicinal materials are more and more diversified. The drying processing of the traditional Chinese medicinal materials is mainly divided into two main categories of a traditional drying method and a processing method utilizing a modern technology, wherein the common traditional drying method of the traditional Chinese medicinal materials comprises a sun drying method, a shade drying method and a drying method; modern drying processing technologies include solar drying, far infrared drying, microwave drying, vacuum freeze drying, forced air drying, vacuum drying, microwave drying, and the like. With the continuous intervention of modern drying methods in the field of processing of Chinese medicinal materials, the drying of Chinese angelica medicinal materials also adopts the modern drying technology.
The required temperature of vacuum drying is lower, which is beneficial to the retention of most volatile components, and the operation is simple, but the vacuum drying has the defects of longer required time and higher energy consumption. The invention discloses a storage method of angelica sinensis medicinal materials, which comprises the steps of carrying out vacuum drying on the angelica sinensis medicinal materials, strictly controlling the water content and the drying temperature of the angelica sinensis medicinal materials, then placing the angelica sinensis medicinal materials in a closed container, and filling nitrogen and carbon dioxide for storage, thereby effectively ensuring the quality of the angelica sinensis medicinal materials, avoiding mildew and worm damage, and simultaneously greatly prolonging the storage time of the angelica sinensis medicinal materials.
However, in the prior art, regarding the vacuum drying process of the angelica sinensis, the evaluation index of the quality of the angelica sinensis is single and not comprehensive enough, which is not favorable for ensuring the quality of the angelica sinensis.
Disclosure of Invention
In order to solve the technical problems and comprehensively evaluate the quality of the vacuum-dried angelica sinensis medicinal material, the invention provides a vacuum drying method without damaging the effective components of the angelica sinensis, a plurality of representative indexes are selected, an APH (active particle ph) method is established by combining a modern detection technology and a chemometrics method, the quality of the angelica sinensis medicinal material is comprehensively evaluated, and on the basis, the optimal process parameters of the vacuum drying of the angelica sinensis medicinal material are optimized, so that the quality of the angelica sinensis medicinal material is ensured to the greatest extent. The technical scheme of the invention is as follows:
a vacuum drying method without destroying effective components of radix Angelicae sinensis comprises the following steps:
step (1), pretreatment:
removing stems and leaves of the underground part of the fresh picked angelica medicinal material, then washing with clear water to remove silt and surface attachments, cleaning, and draining surface water for later use;
step (2), vacuum drying
Weighing clean fresh angelica medicinal materials at random, putting the fresh angelica medicinal materials into vacuum drying equipment for drying, setting the drying temperature to be 40-80 ℃, and keeping the vacuum pressure to be-0.05-0.10 Mpa in the drying process;
and (3) after drying is finished, stopping heating, discharging after vacuum discharge, and finishing, sealing and storing.
Further, in the step (2), the drying temperature is set to be 60 ℃, and the vacuum pressure is kept to be-0.08 MPa in the drying process.
Further, the angelica medicinal material is dried in vacuum by using the whole angelica or the main root, fibrous root and slices of the angelica.
Further, in the step (2), the drying time is 13-37 h.
Further, the effective components include tryptophan, chlorogenic acid, ferulic acid, senkyunolide I, senkyunolide H, imperatorin, Z-ligustilide, butenyl phthalide, extract and polysaccharide.
The invention is further illustrated by the following experimental studies.
(1) AHP method for evaluating quality of Chinese angelica medicinal material
The evaluation target can be reflected by multi-index components, and the target tree for angelica drying process evaluation is established on the basis of 8 components such as tryptophan and 12 indexes of volatile oil, extract, polysaccharide and drying time. Then, by comparing the relative importance of the uniform level targets, a pairwise comparison matrix is formed. The scoring criteria for each level of the target tree are shown in table 1. The decision priority matrix for 12 entries in the target tree, labeled for comparison, is shown in table 2. The evaluation matrix of the pairwise comparison of 12 indices using yaahp software and table 2 was used to perform a weight analysis to calculate the index composite score (V), see table 3.
TABLE 1 target Tree graph hierarchy Scoring criteria
| Relative importance of | Definition of |
| 1 | Of equal importance |
| 3 | Of |
| 5 | Of obvious importance |
| 7 | Of strong importance |
| 9 | Of absolute importance |
| 2、4、6、8 | Intermediate values of two adjacent degrees, adopted when compromise is required |
TABLE 2 decision priority matrix for pairwise comparisons
TABLE 3 weight ratio table of each component
| Index (I) | Weight coefficient |
| Tryptophan | 0.0145 |
| Chlorogenic acid | 0.0144 |
| Ferulic acid | 0.2534 |
| Senkyunolide I | 0.0890 |
| Senkyunolide H | 0.0479 |
| Imperatorin | 0.0890 |
| Z-ligustilide | 0.1990 |
| Butylene phthalide | 0.0428 |
| Essential oils | 0.0482 |
| Extract of plant | 0.0273 |
| Polysaccharides | 0.0349 |
| Drying time | 0.1394 |
(2) Single factor experiment of vacuum drying process-drying temperature
Weighing fresh angelica medicinal materials randomly, cleaning, placing in a vacuum drying oven for drying, fixing the pressure of a drying chamber to be-0.05 to-0.10 MPa, and selecting 40 ℃, 50 ℃, 60 ℃ and 70 ℃ as investigation factors. And (5) observing the sublimation temperature, and sampling and detecting at different time periods respectively. According to the obtained content detection result, comprehensive scoring is carried out by adopting an AHP method, the moisture change condition of the vacuum drying process is shown in table 4, and the moisture content change graph and the drying rate change graph of the drying process test show that the moisture content of the traditional Chinese medicinal material in the drying process is relatively high in the initial drying stage, and the moisture content is gradually reduced to be gentle when the moisture content is reduced to about 10-15% along with the extension of the drying time, as shown in fig. 1 and 2.
The volatile oil detection results are shown in table 5, the volatile oil content change chart of the vacuum drying process shows that the volatile oil change condition is consistent with the moisture change condition, the volatile oil content gradually decreases along with the extension of the drying time, the initial decrease is faster, and then the volatile oil content gradually tends to be gentle, as shown in fig. 3, the effective component content measurement results are shown in table 6, and the comprehensive scoring results are shown in table 7. And selecting 40-80 ℃ for vacuum drying according to the grading result.
TABLE 4 moisture Change Table of vacuum drying Process
TABLE 5 volatile oil test results Table
TABLE 6 measurement results of the content of active ingredient
TABLE 7 comprehensive scoring results Table
| Process parameters | Drying time/h | Composite score |
| Vacuum drying at 40 deg.c and-0.05-0.10 MPa | 37 | 2.2555 |
| Vacuum drying at 50 deg.C to-0.05-0.10 MPaa | 27 | 2.5595 |
| Vacuum drying at 60 deg.c and-0.05-0.10 MPa | 21 | 3.0658 |
| Vacuum drying at 70 deg.C to-0.05-0.10 MPa | 13 | 3.2201 |
(3) Quality comparison of Chinese angelica obtained by different drying processes
Selecting fresh angelica medicinal materials in the same batch, drying by adopting a traditional drying method, and comparing with the angelica medicinal materials treated by the method. Through observing and detecting the angelica samples with different drying modes, the influence of the different drying modes on the chemical components and the appearance properties of the angelica medicinal material is different. The appearance and cut surface comparison of the angelica medicinal materials with different drying processes are shown in Table 8. The results of the content determination and scoring of the active ingredients are shown in table 9.
TABLE 8 comparative results of appearance and cut surface of radix Angelicae sinensis by different drying processes
TABLE 9 table of determination and evaluation results of effective ingredient content
| Content of active ingredient (%) | Drying by baking | Vacuum drying |
| Tryptophan | 0.1611 | 0.1673 |
| Chlorogenic acid | 0.0243 | 0.0368 |
| Ferulic acid | 0.1191 | 0.1426 |
| Senkyunolide I | 0.0253 | 0.0241 |
| Senkyunolide H | 0.0042 | 0.0038 |
| Imperatorin | 0.4894 | 0.3912 |
| Z-ligustilide | 4.0246 | 4.3847 |
| Butylene phthalide | 0.0599 | 0.0640 |
| Essential oils | 1.05 | 1.05 |
| Extract of plant | 53.67 | 56.58 |
| Polysaccharides | 0.048 | 0.062 |
| Moisture content | 4.98 | 5.02 |
| Drying time/h | 28 | 21 |
| Composite score | 2.6623 | 3.0941 |
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention establishes a scoring system by combining a chemometrics method, researches the angelica vacuum drying process, basically covers the main active ingredients of the angelica medicinal material by the selected evaluation indexes, and effectively and comprehensively evaluates the quality of the angelica medicinal material.
(2) Compared with the traditional drying method, the angelica medicinal material treated by the method effectively ensures that the effective components represented by volatile oil in the angelica medicinal material are not damaged, the appearance of the vacuum-dried angelica is better maintained, the color of the epidermis and the section is lighter than that of the dried angelica and is closer to that of the fresh medicinal material, and the angelica medicinal material can be dried at a lower temperature in a vacuum state, so that the drying time is shorter and the energy is saved. Meanwhile, the method is simple and easy to implement, has strong practicability and is suitable for large-scale production.
(3) The angelica vacuum drying method provided by the invention firstly researches the drying dynamics of angelica medicinal material vacuum drying and the change condition of effective components, adopts the AHP method to carry out weighting grading, carries out overall evaluation on the quality of the angelica medicinal material with different drying process parameters, and preferably selects the optimal process parameter of vacuum drying according to the grading result. Provides reference for improving the quality of the angelica medicinal material and the standardized processing thereof. The vacuum drying method established by the invention has uniform heat transfer, effectively prevents the denaturation of the active ingredients in the angelica medicinal material, well retains the active ingredients represented by volatile oil, and the dried angelica medicinal material has strong smell and compact texture. Compared with the common drying mode, the drying in the vacuum state better maintains the color of the angelica medicinal material, is closer to the fresh medicinal material and saves about 25 percent of time.
Drawings
FIG. 1 is a graph of the change in drying rate for a single factor experiment;
FIG. 2 is a graph showing the variation of the volatile oil content in a single factor experiment;
FIG. 3 is a diagram of vacuum-dried Angelica sinensis;
FIG. 4 is a drawing of dried Angelica sinensis;
FIG. 5 is a sectional view of a vacuum-dried Angelica sinensis;
FIG. 6 is a sectional view of dried Angelica sinensis;
Detailed Description
In order to make the technical solution of the present invention easy to understand, the following is further described with reference to specific examples, but not limited to the present invention. Modifications and improvements may be made without departing from the principles of the invention and are intended to be within the scope of the invention.
Description of the drawings: the content determination method of tryptophan, chlorogenic acid, ferulic acid, senkyunolide I, senkyunolide H, imperatorin, Z-ligustilide and butenyl phthalide in the invention comprises the following steps:
(1) preparation of a test solution: taking about 1.0g of the product powder (passing through a third sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 20mL of 70% methanol, sealing the plug, weighing, heating and refluxing for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking up, standing, taking the supernatant, filtering, and taking the subsequent filtrate.
(2) Preparation of control solutions: accurately weighing appropriate amount of tryptophan, chlorogenic acid, ferulic acid, senkyunolide I, senkyunolide H, imperatorin, Z-ligustilide and butenyl phthalide, adding methanol to prepare solution containing tryptophan 50 μ g, chlorogenic acid 70 μ g, ferulic acid 55 μ g, senkyunolide I16 μ g, senkyunolide H5 μ g, imperatorin 190 μ g, Z-ligustilide 500 μ g and butenyl phthalide 50 μ g per 1ml, and obtaining the final product.
(3) Chromatographic conditions are as follows: c18 (4.6X 150mm, 5 μm) column; the flow rate is 1.0ml/min, and the column temperature is 30 ℃; the detection wavelength is 280 nm; the sample amount is 10 mul; the theoretical plate number is more than 5000; eluting with mobile phase A-acetonitrile and B-0.085% phosphoric acid aqueous solution in a gradient manner for 0-10 min (10% A-90% B), 10-15 min (10% → 12% A-90% → 88% B), 15-20 min (12% → 22% A-88% → 78% B), 20-56 min (22% → 62% A-78% → 38% B), 56-60 min (62% → 70% A-38% → 30% B), 60-65 min (70% → 10% A-30% → 90% B), and 65-70 min (10% A-90% B).
(4) The determination method comprises the following steps: respectively sucking 10 μ L of the mixed reference solution and sample solution, injecting into liquid chromatograph, and measuring.
Example 1
The vacuum drying method for not destroying the effective components of angelica in the embodiment, which is directed at the main root of angelica sinensis in Yunnan Weixi, comprises the following steps:
(1) pretreatment: washing the underground part of the dug Yunnan Weixi fresh Chinese angelica medicinal material with clear water, removing silt and surface attachments, cleaning, and draining the surface water for later use.
(2) Weighing clean fresh radix Angelicae sinensis, and drying in vacuum drying equipment at 40 deg.C under-0.05 MPa for 30 hr.
(3) And after drying is finished, stopping heating, discharging after vacuum discharge, and finishing, sealing and storing.
The detection results and comprehensive scoring results of the content of the active ingredients in the freeze-drying process of the main roots of the Yunnan Weixi Chinese angelica are shown in a table 10.
TABLE 10 table of determination of contents of effective components and evaluation results
According to the scoring result, the method can be stably used for vacuum drying of the angelica sinensis medicinal material.
Example 2
The vacuum drying method for angelica without destroying the effective components of angelica in this embodiment, which is directed at angelica sinensis fibrous root in the irkutsk-maiden, includes the following steps:
(1) pretreatment: and (3) washing the underground part of the dug fresh angelica sinensis medicinal material in the Marima plant with clear water, removing silt and surface attachments, cleaning, and draining surface water for later use.
(2) Weighing clean fresh radix Angelicae sinensis, placing into vacuum drying equipment, drying at 60 deg.C under-0.07 MPa for 15 hr.
(3) And after drying is finished, stopping heating, discharging after vacuum discharge, and finishing, sealing and storing.
The results of the content detection of the active ingredients and the comprehensive scoring results of the vacuum drying process of the radicle of angelica gigantea are shown in table 11.
TABLE 11 table of determination of contents of effective components and evaluation results
According to the scoring result, the method can be stably used for vacuum drying of the angelica sinensis medicinal material.
Example 3
The vacuum drying method for not destroying the effective components of angelica sinensis in this embodiment, which is specific to the whole classification of angelica sinensis in Gansu, includes the following steps:
(1) pretreatment: and (3) washing the underground part of the collected Gansu fresh Chinese angelica medicinal material with clear water, removing silt and surface attachments, cleaning, and draining surface water for later use.
(2) Weighing clean fresh angelica at random, cutting into slices of 2-3 mm, putting into vacuum drying equipment for drying, setting the drying temperature at 80 ℃, keeping the vacuum pressure at-0.10 MPa in the drying process, and keeping the drying time at 2 hours.
(3) And after drying is finished, stopping heating, discharging after vacuum discharge, and finishing, sealing and storing.
The results of the content detection of the active ingredients in the Gansu angelica slices by the vacuum drying process and the comprehensive scoring results are shown in Table 12.
TABLE 12 table of determination and evaluation results of effective ingredient content
According to the scoring result, the method can be stably used for vacuum drying of the angelica sinensis medicinal material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A vacuum drying method without damaging the effective components of angelica sinensis is characterized in that: the method comprises the following steps:
pretreatment in step (1):
removing stems and leaves of the underground part of the fresh picked angelica medicinal material, then washing with clear water to remove silt and surface attachments, cleaning, and draining surface water for later use;
step (2), vacuum drying
Weighing clean fresh angelica medicinal materials at random, putting the fresh angelica medicinal materials into vacuum drying equipment for drying, setting the drying temperature to be 40-80 ℃, and keeping the vacuum pressure to be-0.05 to-0.10 Mpa in the drying process;
and (3) after drying is finished, stopping heating, discharging after vacuum discharge, and finishing, sealing and storing.
2. The vacuum drying method of claim 1, which does not destroy the effective components of Angelica sinensis, comprising: in the step (2), the drying temperature is set to be 60 ℃, and the vacuum pressure is kept to be-0.08 MPa in the drying process.
3. The vacuum drying method of claim 1, which does not destroy the effective components of Angelica sinensis, comprising: the angelica medicinal material is vacuum dried with angelica or angelica root, fibrous root and slice.
4. The vacuum drying method of claim 1, which does not destroy the effective components of Angelica sinensis, comprising: in the step (2), the drying time is 13-37 h.
5. The vacuum drying method of claim 1, which does not destroy the effective components of Angelica sinensis, comprising: the effective components include tryptophan, chlorogenic acid, ferulic acid, senkyunolide I, senkyunolide H, imperatorin, Z-ligustilide, butenyl phthalide, extract and polysaccharide.
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Application publication date: 20200915 |