WO2019104972A1 - 一种山核桃油的微胶囊化工艺 - Google Patents

一种山核桃油的微胶囊化工艺 Download PDF

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Publication number
WO2019104972A1
WO2019104972A1 PCT/CN2018/089106 CN2018089106W WO2019104972A1 WO 2019104972 A1 WO2019104972 A1 WO 2019104972A1 CN 2018089106 W CN2018089106 W CN 2018089106W WO 2019104972 A1 WO2019104972 A1 WO 2019104972A1
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Prior art keywords
wall material
mass ratio
pecan oil
oil
liquid
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PCT/CN2018/089106
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English (en)
French (fr)
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江勇
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深圳市聚尘科技有限公司
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Publication of WO2019104972A1 publication Critical patent/WO2019104972A1/zh

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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up

Definitions

  • the present invention relates to the field of microencapsulation technology of products, and in particular to a microencapsulation process of pecan oil.
  • Pecan is the fruit of the genus Pecans of the genus Juglans, also known as walnut carp and walnut pupa, mainly distributed in the mountainous areas of Hunan, Guizhou, Jiangxi, Zhejiang and other provinces in China.
  • Pecan kernel is rich in protein, fat, total sugar, crude fiber, various mineral elements and vitamins, including fat content of 50% - 64%, protein content of 15-20%, sugar content of about 10%.
  • Pecan oil can be prepared from the fat in pecans.
  • the main component is unsaturated fatty acid, especially linoleic acid and linolenic acid (the linoleic acid content is 71%, the linolenic acid content is 12%).
  • pecan oil has a wide range of uses, and can be used as industrial high-grade lubricating oil, raw materials for cosmetics, and skin burns for external use.
  • Microcapsule technology is a process in which a solid, liquid or gas-coated substance is wrapped in a tiny translucent or closed capsule by special means.
  • the capsule is approximately spherical and generally has a diameter of 5 to 500 (X111. It can be simply regarded as consisting of a heart material and a wall material, the heart material is the material to be encased, and the wall material is the embedding material.
  • oils such as salad oil, fish oil, and flavors such as ginger oil, peppermint oil, and cream have been successfully embedded, but the microencapsulation of pecan oil has rarely been reported in China.
  • the main object of the present invention is to compensate for the above problems, and to provide a microencapsulation process of pecan oil with simple process, long-term stability and high embedding rate.
  • the present invention provides a microencapsulation process for pecan oil, which is characterized in that it comprises the following steps:
  • the wall material is prepared: the gum arabic is weighed according to the mass ratio 1: 2 - 4: 2 - 4, (3 - cyclodextrin and maltodextrin are mixed as a wall material, dissolved in 65-70 ° ( : In the water, after stirring until completely dissolved, it is filtered with gauze to collect the filtrate; wherein, according to the mass of the wall material, the mass of water to be dissolved in the wall material is 4-6 ⁇ ;
  • centrifugal spray drying the above homogenized mixture is allowed to stand 20-40111111 and then spray dried; the condition is: the inlet air temperature is 200-220 ° (:, the outlet air temperature is 70-85 ° (: , centrifuge speed 800 ⁇ ] ⁇ /! ⁇ , feed rate
  • the emulsifier in step 310 is a monoglyceride or sucrose fatty acid ester having a mass ratio of 1:1.
  • step 320 the mass ratio of gum arabic, (3-cyclodextrin and maltodextrin 1: 4:4).
  • the invention has simple formula, simple process, long-term stability, high embedding rate, and the prepared pecan oil microcapsule is non-toxic and convenient to use, and is suitable for direct application in food, health care products, cosmetics and the like. .
  • the present invention provides a microencapsulation process for pecan oil, which comprises the following steps:
  • pecan oil is a non-polar compound and insoluble in water.
  • an emulsifier is essential.
  • the oil-in-water emulsifier should be selected.
  • the oil-in-water emulsifier has a mass ratio of 1: 1 monoglyceride and sucrose fatty acid ester.
  • the wall material is prepared: the gum arabic is weighed according to the mass ratio 1: 2 - 4: 2-4, (3 - cyclodextrin and maltodextrin are mixed as a wall material, dissolved in 65-70 ° ( : In the water, after stirring until completely dissolved, it is filtered with gauze to collect the filtrate; wherein, according to the mass of the wall material, the mass of water to be dissolved in the wall material is 4-6 ⁇ ;
  • the size of the microcapsules in the pre-homogeneous system is not uniform, and the particles collide with each other to form flocculation. After homogenization, the particles become smaller by the action of high shear force, the particle size distribution is relatively uniform, and the stability of the emulsion is further improved. , thereby increasing the efficiency of the microencapsulated product.
  • the pecan oil flows at a high speed under a high pressure through a narrow gap, and is simultaneously subjected to a combination of shearing force, impact force, and hole blasting force, and becomes a very fine droplet dispersed in the liquid. . At 50 ° (:, the emulsification and homogenization effect are the best.
  • centrifugal spray drying the above homogenized mixture is allowed to stand 20-40111111 and then spray dried; the condition is: the inlet air temperature is 200-220 ° (:, the outlet air temperature is 70-85 ° (: , centrifuge speed 800 ⁇ ] ⁇ /! ⁇ , feed rate
  • the spray-dried microcapsule granulation is to directly contact the embedded emulsion in the spray drying chamber with the hot gas flow, so that the moisture of the solution wall material is instantaneously evaporated and removed, thereby promoting the formation and solidification of the wall film, and finally forming a a granular powder.
  • the homogenized mixture is allowed to stand, and if it is not layered, it can be dried.
  • the flow rate at the time of feeding should be determined according to the mistiness in the drying tower. Generally, it is only necessary to see a misty surround under the nozzle.
  • centrifugal spray drying the above homogenized mixture is allowed to stand after 20111111 and spray-drying; the condition is: the inlet air temperature is 220 ° (:, the outlet air temperature is 85 ° (:, the centrifuge speed is 800 ⁇ ) ]"/11 ⁇ 11, feed rate 4 ⁇ 1 ⁇ / 111111;
  • centrifugal spray drying the above homogenized mixture is allowed to stand for 40111111 and then spray-dried; the condition is: the inlet air temperature is 200 ° (:, the outlet air temperature is 70 ° (:, the centrifuge speed is 800 ⁇ ) ]"/11 ⁇ 11, feed rate 4011117 ⁇ 0 2019/104972 ⁇ (:17 ⁇ 2018/089106
  • Odor It has the natural aroma of walnut, soft and odorless.
  • Microbial indicators Coliform (approximate number)
  • pathogens not detected Coliform (approximate number)
  • the amount of surface content measured by the n-hexane washing method accurately weigh 1 ⁇ (accurate to 0.0001)
  • the encapsulated pecan oil sample was placed in a Buchner funnel with a diameter of 1 ,. At the same time of suction filtration, the sample was washed with 3 ⁇ 11 hexane, and the washing filtrate was collected to recover n-hexane. Oil quality score.
  • Embedding rate [(oil content - surface oil mass fraction) / oil content] ⁇ 100%
  • the microencapsulated pecan oil prepared by the invention has a water content of 2.5%-5.4%, a particle size of 30-120%, an embedding rate of 76.5%-86.4%, and an oil content of 35%. — 38%, the microencapsulation efficiency of the product was determined to be 84.2%.
  • the antioxidant stability of the pecan oil was significantly improved after embedding. At room temperature, the shellfish could survive 8-10 (1, the peroxide value increased by 0.5- 0.58
  • the invention has simple formula, simple process, long-term stability, high embedding rate, and the prepared pecan oil microcapsule can be directly used as a nutritious food additive, and expands the pecan oil in the food industry.
  • the application range is more convenient, and at the same time, it finds a new way for the deep processing of pecans.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Cosmetics (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

一种山核桃油的微胶囊化工艺,包括配料、配制壁材、均质、离心喷雾干燥、过筛等步骤。质量比1:2-4:2-4的阿拉伯胶、β-环糊精以及麦芽糊精混合后作为壁材。

Description

\¥0 2019/104972 卩(:17 \2018/089106
一种山核桃油的微胶囊化工艺
技术领域
[0001] 本发明涉及产品的微胶囊化技术领域, 特别涉及一种山核桃油的微胶囊化工艺 背景技术
[0002] 山核桃为胡桃科山核桃属植物果实, 又叫核桃楸、 胡桃楸, 主要分布在我国湖 南、 贵州、 江西、 浙江等省的山区。 山核桃仁含有丰富的蛋白质、 脂肪、 总糖 、 粗纤维、 多种矿物质元素和维生素等营养成分, 其中脂肪含量 50%— 64%, 蛋 白质含量 15— 20%, 糖分含量 10%左右。 山核桃油可由山核桃中的脂肪制备而来 , 主要成分为不饱和脂肪酸, 特别以亚油酸和亚麻酸为主 (亚油酸含量达到 71 % , 亚麻酸含量为 12%) , 长期食用可防止动脉硬化, 减少心脏发病率, 有利 于智力发育, 是一种很好的保健食用油。 山核桃油除食用外还有比较广泛的用 途, 可以作为工业高档润滑油, 化妆品的原料, 皮肤烧伤外用药等。
[0003] 由于山核桃油中不饱和脂肪酸很高, 山核桃油很容易氧化, 造成营养的损失和 品质下降。 为了防止油脂氧化, 同时方便贮存、 运输及使用, 人们发明了微胶 囊
Figure imgf000002_0001
技术。 微胶囊技术又称微胶囊化, 它是用特殊手段将 固体、 液体或气体等需要包被的物质包裹在一微小的半透明或封闭胶囊内的过 程。 胶囊近似球形, 直径一般为 5— 500(X111。 可简单地看作由心材和壁材组成, 心材即被包物质, 壁材即包埋物质。
[0004] 目前国内已经成功地对色拉油、 鱼油等油脂以及姜油、 薄荷油、 奶油等香精香 料实现了包埋, 但对山核桃油的微胶囊化国内鲜见报道。
技术问题
[0005] 本发明的主要目的是为了弥补上述问题, 提出一种工艺简便、 久置稳定、 包埋 率高的山核桃油的微胶囊化工艺。
问题的解决方案
技术解决方案 \¥0 2019/104972 卩(:17 \2018/089106
[0006] 本发明提出一种山核桃油的微胶囊化工艺, 其特征在于, 包括如下步骤:
[0007] 810, 配料: 按质量比 5:1称取山核桃油和乳化剂, 混合后置于 60— 70° (:条件下 搅拌 15-201^!!得到料液, 保持温度备用;
[0008] 820, 配制壁材: 按质量比 1 : 2—4: 2— 4称取阿拉伯胶、 (3 -环糊精及麦芽糊精 混合后作为壁材, 溶于 65— 70° (:的水中, 搅拌均匀至完全溶解后, 用纱布过滤, 收集滤液; 其中, 以所述壁材的质量计, ^壁材需溶入的水的质量为 4一 6§ ;
[0009] 830, 均质: 取一定量步骤 320得到的滤液缓慢加入步骤 310得到的料液中得到 混合液, 使用剪切乳化搅拌机搅拌所述混合液 15— 2011^11后在 50° (:、 40MPa压力 下均质 2次; 其中, 按质量比计算, 滤液: 料液 =1.5: 1 ;
[0010] 840, 离心喷雾干燥: 将上述均质后的混合液静置 20— 40111111后进行喷雾干燥; 条件是: 进风温度为 200— 220° (:, 出风温度 70— 85° (:, 离心机转速 800〇]·/!^, 进料速度
Figure imgf000003_0001
[0011] 850, 过筛: 将上述经喷雾干燥的产品过 80目筛, 即得山核桃油微胶囊产品。
[0012] 优选地, 步骤 310中所述乳化剂为质量比为 1:1的单甘脂、 蔗糖脂肪酸酯。
[0013] 优选地, 步骤 320中阿拉伯胶、 (3 -环糊精及麦芽糊精的质量比 1 : 4: 4。
发明的有益效果
有益效果
[0014] 本发明配方简单, 工艺简便、 久置稳定, 包埋率高, 制成的山核桃油微胶囊具 有无毒、 使用方便等特点, 适用于食品、 保健品、 化妆品等领域的直接应用。 实施该发明的最佳实施例
本发明的最佳实施方式
[0015] 应当理解, 此处所描述的具体实施例仅仅用以解释本发明, 并非用于限定本发 明的范围。
[0016] 本发明提出一种山核桃油的微胶囊化工艺, 其包括如下步骤:
[0017] 810, 配料: 按质量比 5:1称取山核桃油和乳化剂, 混合后置于 60— 70° (:条件下 搅拌 15-201^!!得到料液, 保持温度备用;
[0018] 山核桃油作为制备微胶囊的芯材, 属于非极性化合物, 不溶于水。 为了使山核 桃油与水溶性壁材混合均匀, 乳化剂的使用必不可少。 为使山核桃油分子高度 \¥0 2019/104972 卩(:17 \2018/089106 分散于料液中, 应选择水包油型乳化剂。 具体地, 本实施中, 所述水包油型乳 化剂为质量比为 1 : 1的单甘脂和蔗糖脂肪酸酯。
[0019] 820 , 配制壁材: 按质量比 1 : 2—4: 2— 4称取阿拉伯胶、 (3 -环糊精及麦芽糊精 混合后作为壁材, 溶于 65— 70° (:的水中, 搅拌均匀至完全溶解后, 用纱布过滤, 收集滤液; 其中, 以所述壁材的质量计, ^壁材需溶入的水的质量为 4一 6§ ;
[0020] 阿拉伯胶作为壁材具有较好的成膜性、 乳化性及囊壁致密性, 但复水性、 溶解 性相对较差; 麦芽糊精具有较高的溶解性, 但囊壁疏松、 成膜性差; (3 -环糊精本 身无毒, 可生物降解, 是一种较理想的包覆材料。 因此在微胶囊的壁材选择上 选择三者复配。 当三者质量比为 1 : 2-4: 2— 4时, 且优选地, 当阿拉伯胶、
(3 -环糊精及麦芽糊精质量比 1 : 4: 4时复配效果最好。 这是由于阿拉伯胶虽然乳 化性、 成膜性好, 能在液滴表面形成一层光滑的膜, 但同时也具增稠性, 如果 比例过高, 易造成料液粘度过大, 不利于离心喷雾时雾滴的形成, 从而降低包 埋率; 麦芽糊精成膜性差,形成的胶囊囊壁疏松, 如果比例过高, 也会降低包埋 率, 而 (3 -环糊精则能较好的均衡。
[0021] 830, 均质: 取一定量步骤 320得到的滤液缓慢加入步骤 310得到的料液中得到 混合液, 使用剪切乳化搅拌机搅拌所述混合液 15— 2011^11后在 50° (:、 40MPa压力 下均质 2次; 其中, 按质量比计算, 滤液: 料液 =1.5: 1 ;
[0022] 均质前体系中的微胶囊颗粒大小不均匀, 颗粒彼此碰撞易形成絮凝, 经过均质 后颗粒受高剪切力作用而变小, 粒子大小分布比较均匀, 乳状液稳定性进一步 提高, 从而提高微胶囊化产品的效率。 具体的, 实际操作中, 山核桃油在高压 下高速流过狭窄的缝隙, 同时受到剪切力、 撞击力和空穴爆炸力等的综合作用 , 变成非常细微的液滴分散于料液中。 且在 50 ° (:时, 乳化、 均质效果最佳。
[0023] 840, 离心喷雾干燥: 将上述均质后的混合液静置 20— 40111111后进行喷雾干燥; 条件是: 进风温度为 200— 220° (:, 出风温度 70— 85° (:, 离心机转速 800〇]·/!^, 进料速度
Figure imgf000004_0001
[0024] 喷雾干燥微胶囊造粒是将包埋好的乳化液在喷雾干燥室内使之与热气流直接接 触, 使溶液壁材的水分瞬间蒸发除去, 促使壁膜的形成与固化, 最终形成一种 颗粒状粉末。 \¥0 2019/104972 卩(:17 \2018/089106
[0025] 实际操作时, 将均质后的混合液静置, 若不分层, 即可进行干燥。 进料时的流 量应根据干燥塔里的雾状情况而定, 一般只要看到喷头下有雾状环绕便可。
[0026] 850, 过筛: 将上述经喷雾干燥的产品过 80目筛, 即得山核桃油微胶囊产品。
[0027]
[0028] 实施例 1 :
[0029] 810, 配料: 称取山核桃油 50(^、 单甘脂 5(^、 蔗糖脂肪酸酯 5(^混合后置于 60
°(:条件下搅拌 20111^得到料液, 保持温度备用;
[0030] 820, 配制壁材: 称取阿拉伯胶 100§、 (3 -环糊精 200§、 麦芽糊精 300§混合后作 为壁材, 溶于 2.4 §、 65° (:的水中, 搅拌均匀至完全溶解后, 用纱布过滤, 收集 滤液;
[0031] 830, 均质: 取步骤 320得到的滤液 90(^缓慢加入步骤 310得到的料液 60(^中得 到混合液, 使用剪切乳化搅拌机搅拌所述混合液 151^!!后在 50° (:、 40MPa压力下 均质 2次;
[0032] 840, 离心喷雾干燥: 将上述均质后的混合液静置 20111111后进行喷雾干燥; 条件 是: 进风温度为 220° (:, 出风温度 85° (:, 离心机转速 800〇]"/11^11, 进料速度 4〇1^/ 111111;
[0033] 850, 过筛: 将上述经喷雾干燥的产品过 80目筛, 即得山核桃油微胶囊产品。
[0034] 实施例 2:
[0035] 810, 配料: 称取山核桃油
Figure imgf000005_0001
单甘脂 10(^、 蔗糖脂肪酸酯 10(^混合后置于 7
0 (:条件下搅拌 15111 得到料液, 保持温度备用;
[0036] 820, 配制壁材: 称取阿拉伯胶 100§、 (3 -环糊精 400§、 麦芽糊精 400§混合后作 为壁材, 溶于 5.4 §、 70° (:的水中, 搅拌均匀至完全溶解后, 用纱布过滤, 收集 滤液;
[0037] 830, 均质: 取步骤 320得到的滤液 1.8 §缓慢加入步骤 310得到的 1.2 §料液中 得到混合液, 使用剪切乳化搅拌机搅拌所述混合液 20111^后在 50° (:、 40MPa压力 下均质 2次;
[0038] 840, 离心喷雾干燥: 将上述均质后的混合液静置 40111111后进行喷雾干燥; 条件 是: 进风温度为 200° (:, 出风温度 70° (:, 离心机转速 800〇]"/11^11, 进料速度 4011117 \¥0 2019/104972 卩(:17 \2018/089106
111111
[0039] 850, 过筛: 将上述经喷雾干燥的产品过 80目筛, 即得山核桃油微胶囊产品。
[0040]
[0041] 对本发明实施例 1一 2制备的山核桃油微胶囊产品进行质量标准检验:
[0042] 色泽: 淡黄色
[0043] 气味: 具有核桃特有的天然香味, 柔和、 无异味。
[0044] 微生物指标:
Figure imgf000006_0001
大肠菌群(近似数) £10个 致病菌没有检出
[0045] 过氧化值测定: 按06 5538-85方法测定;
[0046] 表面油及包埋率测定:
[0047] 正己烷洗涤法测表面含量量: 准确称取 1 § (准确至 0.0001
Figure imgf000006_0002
胶囊化山核桃油 样品平铺于直径为 1〇 的布氏漏斗中, 在抽滤同时, 用 3〇11^正已烷洗涤样品 , 收集洗涤滤液, 回收正已烷, 称洗涤油质量得表面油质量分数。
[0048] 索氏抽提法测总含油量: 将
Figure imgf000006_0004
(准确至 0.0001
Figure imgf000006_0003
胶囊化山核桃油样品用 3〇11^ 的石油醚在 75°(:条件下提取 1211, 收集抽提液, 回收石油醚, 称总油质量得含油 率。
[0049] 表面油质量分数= (洗涂油质量 /样品质量) \100%
[0050] 包埋率 = [ (含油率 -表面油质量分数) /含油率] \100%
[0051] 结果显示, 本发明制备的微胶囊化山核桃油, 含水量为 2.5%— 5.4%, 颗粒粒径 在 30— 120—, 包埋率为 76.5%— 86.4%, 油含量在 35%— 38%, 实验测定该产品 的微胶囊化效率为 84.2%, 包埋后山核桃油的抗氧化稳定性明显提高, 在常温下 可贝亡存 8— 10(1, 过氧化值上升 0.5— 0.58
Figure imgf000006_0005
[0052] 本发明配方简单, 工艺简便、 久置稳定, 包埋率高, 制成的山核桃油微胶囊, 既可直接食用, 又可作为营养食品添加剂, 扩大了山核桃油在食品工业的应用 范围, 应用更为方便, 同时为山核桃的深加工寻找了新的出路。
[0053] 以上所述仅为本发明的较佳实施例, 并不用以限制本发明, 凡在本发明的精神 和原则之内, 所作的任何修改、 等同替换、 改进等, 均应包含在本发明的保护 范围之内。 [0054]

Claims

\¥0 2019/104972 卩(:17 \2018/089106 权利要求书
[权利要求 1] 一种山核桃油的微胶囊化工艺, 其特征在于, 包括如下步骤:
810, 配料: 按质量比 5: 1称取山核桃油和乳化剂, 混合后置于 60— 70 °(:条件下搅拌 15-201^!!得到料液, 保持温度备用;
820, 配制壁材: 按质量比 1 : 2—4: 2— 4称取阿拉伯胶、 (3 -环糊精及 麦芽糊精混合后作为壁材, 溶于 65— 70° (:的水中, 搅拌均匀至完全溶 解后, 用纱布过滤, 收集滤液; 其中, 以所述壁材的质量计,
Figure imgf000008_0001
壁材 需溶入的水的质量为 4一 6§ ;
830, 均质: 取一定量步骤 320得到的滤液缓慢加入步骤 310得到的料 液中得到混合液, 使用剪切乳化搅拌机搅拌所述混合液 15-201^!!后 在 50° (:、 40MPa压力下均质 2次; 其中, 按质量比计算, 滤液: 料液 =
1.5:1;
840, 离心喷雾干燥: 将上述均质后的混合液静置 20— 4011^11后进行 喷雾干燥; 条件是: 进风温度为 200— 220° (:, 出风温度 70— 85° (:, 离 心机转速 800〇17]11111, 进料速度 4011117111111;
850, 过筛: 将上述经喷雾干燥的产品过 80目筛, 即得山核桃油微胶 囊产品。
[权利要求 2] 如权利要求 1所述的山核桃油的微胶囊化工艺, 其特征在于, 步骤 310 中所述乳化剂为质量比为 1: 1的单甘脂、 蔗糖脂肪酸酯。
[权利要求 3] 如权利要求 1所述的山核桃油的微胶囊化工艺, 其特征在于, 步骤 320 中阿拉伯胶、 (3 -环糊精及麦芽糊精的质量比 1 : 4: 4。
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