CN115590864B - Process for preparing high-stability glucosamine sulfate by fermentation method - Google Patents

Process for preparing high-stability glucosamine sulfate by fermentation method Download PDF

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CN115590864B
CN115590864B CN202211222483.0A CN202211222483A CN115590864B CN 115590864 B CN115590864 B CN 115590864B CN 202211222483 A CN202211222483 A CN 202211222483A CN 115590864 B CN115590864 B CN 115590864B
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glucosamine sulfate
decoloring
hydrolysis
stability
fermentation
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CN115590864A (en
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刘长峰
卢健行
韩宁
徐艳
张建华
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Shandong Runde Biotechnology Co Ltd
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    • A—HUMAN NECESSITIES
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    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
    • C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
    • C07H5/06—Aminosugars

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Abstract

The invention discloses a process for preparing high-stability glucosamine sulfate by a fermentation method, which comprises the following steps: (i) Adding sulfuric acid into fermentation liquor prepared by a microbial fermentation method for hydrolysis, and adding alkali liquor into the obtained hydrolysis liquor after the hydrolysis is completed to adjust the hydrolysis liquor to be neutral to obtain the hydrolysis liquor containing glucosamine sulfate. (ii) Adding a decoloring agent into the hydrolysate, decoloring under heating, separating the decoloring agent after the decoloring is finished, and collecting a liquid phase to obtain the decoloring liquid. (iii) Concentrating the decolorized solution, adding sucrose fatty acid ester and corn oil into the obtained concentrated solution, stirring to form emulsion, and spray-drying the emulsion to obtain the glucosamine sulfate powder with the surface coated with the hydrophobic layer. According to the process disclosed by the invention, the hydrophobic agent is coated on the surface of the glucosamine sulfate, so that the moisture absorption capacity of the glucosamine sulfate can be effectively reduced, and the stability of the glucosamine sulfate is improved.

Description

Process for preparing high-stability glucosamine sulfate by fermentation method
Technical Field
The invention relates to the technical field of glucosamine preparation, in particular to a process for preparing high-stability glucosamine sulfate by a fermentation method.
Background
Glucosamine (C) 6 H 13 NO 5 ) Is a substance necessary for the synthesis of proteoglycans in the human articular cartilage matrix, and is usually present in polysaccharides of microbial, animal origin and conjugated polysaccharides. Currently, glucosamine is prepared by hydrolyzing raw materials (such as shrimp shells, crab shells, etc.) containing chitin, and performing microbial fermentation or enzymolysis. The method for hydrolyzing shrimp shell and crab shell requires a large amount of concentrated hydrochloric acid to generate a large amount of waste liquid, which is easy to cause severeThe heavy environmental pollution problem, and the problem that the glucosamine prepared by taking shrimp shells, crab shells and the like as raw materials can cause allergic reaction of allergic constitution patients in the clinical application process. The enzymolysis method has high cost and low production efficiency, and is not suitable for large-scale production and application. The microbial fermentation method has the advantages of no fishy smell, short production period, high yield, little environmental pollution and the like, and becomes a main method for producing the glucosamine. The currently prepared glucosamine mainly exists in the form of hydrochloride or sulfate, the performance of the glucosamine hydrochloride is relatively stable, but the absorption of the glucosamine sulfate in a human body is poor, the absorption of the glucosamine sulfate in the human body is good due to sulfate radical, but the problem of strong hygroscopicity exists, so that the glucosamine sulfate is unstable and deliquescent, and for this reason, generally, 20-30% of the glucosamine hydrochloride is added into the glucosamine sulfate, but the problem of excessively high salt content or chloride ion content of the glucosamine product is caused, and the glucosamine sulfate is not suitable for partial users.
Disclosure of Invention
Aiming at the problems, the invention provides a process for preparing high-stability glucosamine sulfate by a fermentation method, which can effectively reduce the moisture absorption capacity of the glucosamine sulfate and improve the stability of the glucosamine sulfate by coating a layer of hydrophobic film on the surface of the glucosamine sulfate. In order to achieve the above purpose, the present invention discloses the following technical solutions:
a process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) Adding sulfuric acid into fermentation liquor prepared by a microbial fermentation method for hydrolysis, and adding alkali liquor into the obtained hydrolysis liquor after the hydrolysis is completed to adjust the hydrolysis liquor to be neutral to obtain the hydrolysis liquor containing glucosamine sulfate.
(ii) Adding a decoloring agent into the hydrolysate, decoloring under heating, separating the decoloring agent after the decoloring is finished, and collecting a liquid phase to obtain the decoloring liquid.
(iii) Concentrating the decolorized solution, adding sucrose fatty acid ester and corn oil into the obtained concentrated solution, stirring to form emulsion, and spray-drying the emulsion to obtain the glucosamine sulfate powder with the surface coated with the hydrophobic layer.
In a further embodiment, in step (i), the concentration of sulfuric acid is 55 to 65wt.%.
In a further embodiment, in step (i), the sulfuric acid concentration of the system is maintained between 30 and 38wt.% after the sulfuric acid addition. The metabolic products in the fermentation liquor are hydrolyzed by sulfuric acid, so that the glucosamine sulfate can be directly obtained, the introduction of chloride ions is avoided, and the pollution problem caused by massive volatilization during the hydrolysis of concentrated hydrochloric acid can be relieved.
In a further embodiment, in step (i), the hydrolysis is carried out at a temperature of 65 to 85 ℃ for a duration of 3 to 5 hours.
In a further technical scheme, in the step (i), the alkali liquor comprises any one of sodium hydroxide, sodium carbonate, sodium bicarbonate and the like.
In a further embodiment, in step (ii), the decolorizing agent includes any one of activated carbon, diatomaceous earth, and the like. Optionally, the addition amount of the decoloring agent is 3-5 g/L. Preferably, the decoloring is performed under heating at 40-55 ℃ for 20-35 min. The main function of the decoloring agent is to remove pigment in the hydrolysate by physical adsorption, and improve the appearance and purity of the product.
In a further technical scheme, in the step (iii), the decolorized solution is heated and concentrated to 40-60% of the initial volume in a water bath, so that the concentration of glucosamine sulfate in the decolorized solution is increased, and the subsequent spray drying treatment is facilitated.
In a further technical scheme, in the step (iii), 5-7.8 g of sucrose fatty acid ester and 11.2-16 g of corn oil are added into each liter of concentrated solution. The sucrose fatty acid ester has good emulsifying effect on moisture in corn oil and concentrated solution, and emulsion containing glucosamine sulfate is obtained after high-speed stirring.
In a further embodiment, in step (iii), the emulsion is used to prepare the glucosamine sulfate in a spray dryer.
Optionally, the inlet temperature of the spray dryer is 105-115 ℃, the feeding speed is 4-7 mL/min, and then the obtained powder is dried in vacuum for 15-25 min at 50-65 ℃ to obtain the glucosamine sulfate powder.
Compared with the prior art, the invention has the beneficial effects that: in order to overcome the problems of high moisture absorption capacity and unstable and deliquescent property of the glucosamine sulfate, the invention provides a process for preparing the high-stability glucosamine sulfate by a fermentation method. The method comprises the following steps: firstly, the invention directly hydrolyzes the metabolic products in the fermentation liquor by sulfuric acid, which is not only convenient for directly obtaining glucosamine sulfate and avoiding introducing chloride ions, but also is helpful for alleviating pollution caused by massive volatilization during the hydrolysis of concentrated hydrochloric acid. Secondly, the invention directly adds sucrose fatty acid ester and corn oil into the concentrated solution, then stirs to form emulsion, and then spray-dries the emulsion. By the method, after spray drying, the sucrose fatty acid ester and the corn oil are coated on the surface layer of the glucosamine sulfate particles to form a hydrophobic layer, so that the moisture absorption capacity of the glucosamine sulfate is effectively reduced, and the stability of the glucosamine sulfate is improved. Meanwhile, the process also avoids the traditional method of extracting the glucosamine sulfate from the concentrated solution by using an alcohol precipitation method, a large amount of ethanol is added into the concentrated solution to precipitate the glucosamine sulfate in the concentrated solution, then the glucosamine sulfate is separated, the rest liquid phase is waste liquid containing a large amount of ethanol, the waste liquid also faces the problem of subsequent recycling, the process complexity and the cost are increased, and the process of the invention directly adds sucrose fatty acid ester and corn oil into the concentrated solution and then carries out spray drying treatment, thus the problem of the waste liquid is well avoided without adopting the alcohol precipitation method, and the high-stability glucosamine sulfate with the surface coated with a hydrophobic layer is obtained.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. The invention will now be further illustrated by means of a specific implementation.
The preparation method of the fermentation broth in the following examples adopts the following processes: the culture medium in the fermentation tank is 25g/L of glucose, 20g/L of yeast extract powder, 5.5g/L of glycerol, 3g/L of lactose, 3g/L of sodium nitrate, 1g/L of dipotassium hydrogen phosphate, 0.53g/L of magnesium sulfate, 0.11g/L of sodium chloride and 0.03g/L of ferrous sulfate. Then inoculating engineering bacteria (escherichia coli, saccharomyces cerevisiae and staphylococcus which are mixed according to the volume ratio of 3:0.6:1.5) into the fermentation tank for fermentation culture, setting the culture temperature in the fermentation tank to be 37 ℃, setting the culture time to be 45h, adjusting the feeding speed of glucose to be 3.8L/h, filtering the obtained fermentation liquor after completion, removing thalli and the like, and collecting the obtained filtrate for standby. Other suitable fermentation methods can be used to prepare the fermentation broth according to actual needs, and the technology is widely applied in the field.
Example 1
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution with a concentration of 60wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 36wt.%, followed by thermal hydrolysis for 4.5 hours, the heating temperature being maintained at 75.+ -. 2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium hydroxide to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding activated carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 4g/L, decoloring for 30min at 45 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) Heating and concentrating the decolorized solution in water bath to 40% of the initial volume to obtain concentrated solution. Then 5g of sucrose fatty acid ester and 11.2g of corn oil were added to each liter of the concentrate, followed by mechanical stirring at 600 rpm for 3 minutes to form an emulsion.
(iv) And (3) placing the emulsion in a spray dryer for spray drying treatment to prepare the glucosamine sulfate powder. The inlet temperature of the spray dryer is 110 ℃, the feeding speed is 5mL/min, and then the obtained powder is dried in vacuum for 20min at 60 ℃ to obtain the glucosamine sulfate powder.
Example 2
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution having a concentration of 55wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 30wt.%, followed by thermal hydrolysis for 3 hours, the heating temperature being maintained at 85±2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium carbonate to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding active carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 5g/L, decoloring for 20min at 40 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) And heating and concentrating the decolorized solution to 55% of the initial volume in a water bath to obtain a concentrated solution. Then 6.5g of sucrose fatty acid ester and 14g of corn oil were added to each liter of the concentrate, followed by mechanical stirring at 600 rpm for 3 minutes to form an emulsion.
(iv) And (3) placing the emulsion in a spray dryer for spray drying treatment to prepare the glucosamine sulfate powder. The inlet temperature of the spray dryer is 115 ℃, the feeding speed is 7mL/min, and then the obtained powder is dried in vacuum for 15min at 65 ℃ to obtain the glucosamine sulfate powder.
Example 3
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution having a concentration of 65wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 38wt.%, followed by thermal hydrolysis for 5 hours, the heating temperature being maintained at 65±2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium bicarbonate to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding active carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 3g/L, decoloring for 35min at 55 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) And heating and concentrating the decolorized solution to 60% of the initial volume in a water bath to obtain a concentrated solution. Then 7.8g of sucrose fatty acid ester and 16g of corn oil were added to each liter of the concentrate, followed by mechanical stirring at 600 rpm for 5 minutes to form an emulsion.
(iv) And (3) placing the emulsion in a spray dryer for spray drying treatment to prepare the glucosamine sulfate powder. The inlet temperature of the spray dryer is 105 ℃, the feeding speed is 4mL/min, and then the obtained powder is dried in vacuum at 50 ℃ for 25min, so that the glucosamine sulfate powder is obtained.
Example 4
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution with a concentration of 60wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 36wt.%, followed by thermal hydrolysis for 4.5 hours, the heating temperature being maintained at 75.+ -. 2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium hydroxide to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding activated carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 4g/L, decoloring for 30min at 45 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) Heating and concentrating the decolorized solution in water bath to 40% of the initial volume to obtain concentrated solution. And adding ethanol (the mass concentration is 95%) with the volume of 5 times of the concentrated solution for alcohol precipitation, centrifuging (the speed is 10000 r/min, the time is 15 min) to separate out precipitated glucosamine sulfate crystals, and vacuum drying at 60 ℃ for 20min to obtain the glucosamine sulfate.
Example 5
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution having a concentration of 55wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 30wt.%, followed by thermal hydrolysis for 3 hours, the heating temperature being maintained at 85±2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium carbonate to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding active carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 5g/L, decoloring for 20min at 40 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) And heating and concentrating the decolorized solution to 55% of the initial volume in a water bath to obtain a concentrated solution. Then 6.5g of sucrose fatty acid ester was added to each liter of the concentrate, followed by mechanical stirring at 600 rpm for 3 minutes to form an emulsion.
(iv) And (3) placing the emulsion in a spray dryer for spray drying treatment to prepare the glucosamine sulfate powder. The inlet temperature of the spray dryer is 115 ℃, the feeding speed is 7mL/min, and then the obtained powder is dried in vacuum for 15min at 65 ℃ to obtain the glucosamine sulfate powder.
Example 6
A process for preparing high-stability glucosamine sulfate by a fermentation method comprises the following steps:
(i) A sulfuric acid solution having a concentration of 65wt.% was added to the fermentation broth prepared by the above microbial fermentation method until the sulfuric acid concentration in the fermentation broth reached 38wt.%, followed by thermal hydrolysis for 5 hours, the heating temperature being maintained at 65±2 ℃. Filtering the obtained hydrolysate after completion, and then adding sodium bicarbonate to neutralize the hydrolysate to be neutral, thus obtaining the neutral hydrolysate containing glucosamine sulfate.
(ii) Adding active carbon as a decoloring agent into the neutral hydrolysate according to the adding amount of 3g/L, decoloring for 35min at 55 ℃, centrifuging (the speed is 10000 r/min, the time is 15 min) after the completion of the decoloring, separating the decoloring agent from the hydrolysate, and collecting a liquid phase to obtain the decoloring liquid.
(iii) And heating and concentrating the decolorized solution to 60% of the initial volume in a water bath to obtain a concentrated solution. 16g of corn oil per liter of concentrate was then added and then mechanically stirred at 600 revolutions per minute for 5 minutes to form an emulsion.
(iv) And (3) placing the emulsion in a spray dryer for spray drying treatment to prepare the glucosamine sulfate powder. The inlet temperature of the spray dryer is 105 ℃, the feeding speed is 4mL/min, and then the obtained powder is dried in vacuum at 50 ℃ for 25min, so that the glucosamine sulfate powder is obtained.
The moisture absorption rate of the glucosamine sulfate finally obtained in each example was tested by the following method: 50g of the glucosamine sulfate was taken and allowed to stand in a ventilated and light-protected environment for one week, then the weight thereof was tested, and the change relative to the initial weight was calculated, and the results were shown below. It can be seen that the moisture absorption rate of the glucosamine sulfate prepared by the process of examples 1-3 is significantly lower than that of examples 4-6, because the process of examples 1-3 can coat the surfaces of the glucosamine sulfate particles with hydrophobic films, the moisture absorption capacity of the glucosamine sulfate is effectively reduced, and the stability of the glucosamine sulfate is improved. Whereas the conventional alcohol precipitation method adopted in example 4 extracts glucosamine sulfate from the concentrated solution, the obtained glucosamine sulfate has strong hygroscopicity, and is easily deliquesced by water absorption in the air, examples 5 and 6 failed to successfully prepare an effective hydrophobic film on the surface of the glucosamine sulfate particles, resulting in that the hygroscopicity of the obtained glucosamine sulfate is not effectively overcome.
Results of moisture absorption test of glucosamine sulfate
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Moisture absorption rate/% 0.26 0.17 0.21 7.58 6.82 7.04
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. A process for preparing high-stability glucosamine sulfate by a fermentation method is characterized by comprising the following steps:
(i) Adding sulfuric acid into fermentation liquor prepared by a microbial fermentation method for hydrolysis, and adding alkali liquor into the obtained hydrolysis liquor after the hydrolysis is completed to adjust the hydrolysis liquor to be neutral to obtain hydrolysis liquor containing glucosamine sulfate;
(ii) Adding a decoloring agent into the hydrolysate, decoloring under a heating condition, separating the decoloring agent after the decoloring is finished, and collecting a liquid phase to obtain a decoloring liquid;
(iii) Concentrating the decolorized solution, adding sucrose fatty acid ester and corn oil into the obtained concentrated solution, stirring to form emulsion, and spray-drying the emulsion to obtain glucosamine sulfate powder coated with a hydrophobic layer on the surface;
in the step (i), the concentration of sulfuric acid is 55-65wt%;
in the step (i), the sulfuric acid concentration of the sulfuric acid added system is 30-38 wt.%;
in the step (i), the temperature of the hydrolysis is 65-85 ℃ and the duration time is 3-5 hours;
in the step (iii), 5-7.8 g of sucrose fatty acid ester and 11.2-16 g of corn oil are added into each liter of concentrated solution.
2. The process for preparing high-stability glucosamine sulfate by fermentation according to claim 1, wherein in the step (i), the alkali solution comprises any one of sodium hydroxide, sodium carbonate and sodium bicarbonate.
3. The process for preparing high-stability glucosamine sulfate by fermentation according to claim 1, wherein in the step (ii), the decoloring agent comprises any one of activated carbon and diatomite; the addition amount of the decoloring agent is 3-5 g/L; the decoloring is performed under the heating condition of 40-55 ℃ for 20-35 min.
4. The process for preparing high-stability glucosamine sulfate by fermentation according to claim 1, wherein in the step (iii), the decolorized solution is heated and concentrated in a water bath to 40-60% of the initial volume.
5. The process for preparing high stability glucosamine sulfate by fermentation according to any one of claims 1-4, wherein in step (iii), the emulsion is used for preparing the glucosamine sulfate powder in a spray dryer.
6. The process for preparing high-stability glucosamine sulfate by using the fermentation method according to claim 5, wherein the inlet temperature of the spray dryer is 105-115 ℃, the feeding speed is 4-7 mL/min, and the obtained powder is dried in vacuum at 50-65 ℃ for 15-25 min to obtain the glucosamine sulfate powder.
CN202211222483.0A 2022-10-08 2022-10-08 Process for preparing high-stability glucosamine sulfate by fermentation method Active CN115590864B (en)

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Publication number Priority date Publication date Assignee Title
CN1768758A (en) * 2005-11-08 2006-05-10 宛六一 Soft capsule of medicinal composition and its preparation method
CN113402572A (en) * 2021-06-18 2021-09-17 山东润德生物科技有限公司 Process for refining glucosamine composite salt prepared by microbial fermentation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1768758A (en) * 2005-11-08 2006-05-10 宛六一 Soft capsule of medicinal composition and its preparation method
CN113402572A (en) * 2021-06-18 2021-09-17 山东润德生物科技有限公司 Process for refining glucosamine composite salt prepared by microbial fermentation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
生物相容微乳液的构筑及载药研究;董爽爽;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》(第2期);第B014-815页 *

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