CN102294033B - Production process of spherical lactose particle - Google Patents
Production process of spherical lactose particle Download PDFInfo
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- CN102294033B CN102294033B CN 201010209359 CN201010209359A CN102294033B CN 102294033 B CN102294033 B CN 102294033B CN 201010209359 CN201010209359 CN 201010209359 CN 201010209359 A CN201010209359 A CN 201010209359A CN 102294033 B CN102294033 B CN 102294033B
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- Prior art keywords
- lactose
- spherical
- particle
- water crystallization
- production technology
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 title claims abstract description 83
- 239000008101 lactose Substances 0.000 title claims abstract description 83
- 239000002245 particle Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000011248 coating agent Substances 0.000 claims abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 78
- 238000002425 crystallisation Methods 0.000 claims description 32
- 230000008025 crystallization Effects 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 20
- 238000007907 direct compression Methods 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 13
- 239000008187 granular material Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 229930195727 α-lactose Natural products 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007667 floating Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 4
- 150000004682 monohydrates Chemical class 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 14
- 239000000203 mixture Substances 0.000 description 8
- 235000019359 magnesium stearate Nutrition 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 6
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000003814 drug Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- -1 hydroxypropyl Chemical group 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- GUBGYTABKSRVRQ-DCSYEGIMSA-N Beta-Lactose Chemical compound OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-DCSYEGIMSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 239000005862 Whey Substances 0.000 description 1
- 102000007544 Whey Proteins Human genes 0.000 description 1
- 108010046377 Whey Proteins Proteins 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002597 lactoses Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- 229930195724 β-lactose Natural products 0.000 description 1
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- Medicinal Preparation (AREA)
Abstract
The invention relates to a production method of lactose and provides a production process of spherical lactose particles. The production process comprises the following steps of: selecting lactose crystal monohydrate, grinding the lactose crystal monohydrate into particles with particle size range of 38-80Mum to be taken as base stock, taking lactose aqueous solution dissolved with 20-45g of the lactose crystal monohydrate in every 100g of water as coating solution, and coating the particles by adopting a fluidized bed to prepare the spherical lactose particles. The spherical lactose particles prepared by adopting the production process provided by the invention have excellent fluidity and can be applicable to direct powder tabletting in the pharmaceutical industry.
Description
Technical field
The present invention relates to the production method of lactose, be specially the production technology of spherical lactose particle.
Background technology
Lactose makes by extracting in the bovine whey, exists with two kinds of anomer forms, and namely α and β type are respectively monohydrate and anhydride.Alpha-lactose is by making in crystallization below 93.5 ℃ in the supersaturated solution, and beta lactose then is to prepare when being higher than this temperature.Pharmaceutical lactose is modal to be a water crystallization alpha-lactose, makes the product of the different-grain diameters such as 100 orders, 200 orders after sieving by grinding.Because this lactose particle diameter is thin, and crystal formation is rhombus, taper and axe shape etc., poor fluidity.
Lactose is a kind of good tablet filler, uses very extensively in pharmaceuticals industry, and compressibility is good, stable in properties, and with most drug chemically reactive not, the tablet that is pressed into is bright and clean attractive in appearance.
Adopting high speed tablet press is a trend of pharmaceutical preparation without granulation direct pressing tablet, but it is well mobile that this technological requirement tabletting will have with material, the guarantee tablet machine is in situation about running up, material can be filled into pressing mold uniformly, and product sheet behind the tabletting and the weight differential between the sheet are controlled in the acceptability limit.One water crystallization alpha-lactose particle diameter is little, poor fluidity, can't be used for direct compression; can only be by with after active constituents of medicine mixes; make first a certain size wet granular with the granulator wet method, then use oven for drying, make the granule of certain particle diameter, good fluidity and just can suppress in flakes.This technique is loaded down with trivial details, and has increased the unstability to the humidity and temperature sensitive medicaments.
Summary of the invention
The objective of the invention is to be not suitable for the defective of direct compression for a water crystallization lactose poor fluidity, a kind of production technology of spherical, particle diameter bulky grain lactose is provided, the lactose of this explained hereafter has good flowability, especially is fit to quick direct compression.
Technical scheme of the present invention is as follows:
A kind of production technology of spherical lactose particle comprises the following steps:
Get a water crystallization lactose, grind to form the granule of 38～80 μ m particle size ranges, as base material, the lactose aqueous solution of dissolving 20-45g one water crystallization lactose uses fluid bed to carry out granule coating as coating solution in every 100g water again, makes spherical lactose particle.
Wherein, as the lactose of base material and the lactose of preparation lactose solution, it feeds intake is 1～2.3: 1 by weight.
When described lactose aqueous solution prepares, a water crystallization lactose of 20～45 weight portions is dissolved in 65～80 ℃ of deionized waters of 100 weight portions, is stirred to fully dissolving, then be cooled to 30～45 ℃.
The granule coating of carrying out described use fluid bed adopts end spray mode, and the inlet temperature of fluid bed is 50～80 ℃; Temperature of charge is 35～60 ℃.
In the described lactose production technology, after the granule coating, continue to blow floating with 20～35 ℃ of air that dehumidify, relative air humidity is controlled at below 40%, and makes material under fluidized state, evaporates moisture content.The above-mentioned time that blows floating and seethe with excitement was about about 30 minutes.
Further, a described water crystallization lactose is a water crystallization alpha-lactose.
The present invention also provides a kind of lactose flowability that improves to be applicable to the method for direct compression, for adopting above-mentioned technique one water crystallization lactose is processed into spherical lactose particle.
The present invention also further provides a kind of lactose that is applicable to direct compression, is the spherical lactose particle that is prepared by above-mentioned technique.
Spherical lactose particle of the present invention has good size and distribution, has fabulous flowability, can be used for quick tablet machine direct compression, and the product tablet weight variation that suppresses, lustrous surface etc. all can meet the requirements.
The invention has the beneficial effects as follows: a kind of good mobile lactose that has is provided, can be used for the direct pressed powder of pharmaceuticals industry.
The specific embodiment
The present invention will be described below in conjunction with specific embodiment, and should understand example is not for restriction protection scope of the present invention.
The evaluation methodology of adopting among the embodiment:
Powder fluidity: the flowability of powder body is larger on weight differential and the normal operating impact of the preparations such as granule, capsule, tablet, for direct compression, more requires to have higher flowability.The flowability of powder body can't be expressed with single characteristic value, expression angle of repose (angle of repose, θ) commonly used.Refer to free inclined-plane and the formed maximum angular of horizontal plane of powder body accumulation horizon angle of repose.Angle of repose is less, and frictional force is less, and flowability is better, it is generally acknowledged good fluidity when θ≤30 are spent, and can satisfy the need for liquidity in the production process when θ≤40 are spent.
Tablet weight variation: generally guarantee the consistent of every middle active constituent content by control strip with weight differential between the sheet in the production.Inspection method and limit are: get 20 of test samples, accurately weighed gross weight, after trying to achieve average sheet weight, distinguish again accurately weighed every weight, every weight and designation card heavy phase be (without the heavy tablet of designation card, with average sheet anharmonic ratio) relatively, by the regulation in the table, what exceed limit test of weight variation must not be more than 2, and 1 times of 1 overrun must not be arranged.
Lustrous surface: visualization
Frangible degree: get 10 of oral cavity quick disintegrating slices, place tablet friability somascope, rotate 100 times, take out and observe.
Embodiment 1
Get 100 orders, one water crystallization lactose 0.65kg, add the deionized water of 3.25kg, and be heated to 65 ℃, stir and make dissolving.Then cool to 30 ℃.Other gets 100 orders, one water crystallization lactose 1.5kg, crosses 180 orders (80 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 50 degree, and temperature of charge is set to 35 degree.The material preheating begins hydrojet coating, powder coating time 2 h after 10 minutes.Then regulate inlet temperature to 20 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 1.94kg, yield is 90.2%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC (hydroxypropyl emthylcellulose) 35g
Magnesium stearate 15g
5000
Check result is as follows
Embodiment 2
Get 100 orders, one water crystallization lactose 0.65kg, add the deionized water of 3.25kg, and be heated to 80 ℃, stir and make dissolving.Then cool to 45 ℃.Other gets 100 orders, one water crystallization lactose 1.5kg, crosses 400 orders (38 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 80 degree, and temperature of charge is set to 60 degree.The material preheating begins hydrojet coating, powder coating time 2 h after 10 minutes.Then regulate inlet temperature to 35 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 1.88kg, yield is 87.4%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC 35g
Magnesium stearate 15g
5000
Check result is as follows
Embodiment 3
Get 100 orders, one water crystallization lactose 0.65kg, add the deionized water of 1.44kg, and be heated to 75 ℃, stir and make dissolving.Then cool to 35 ℃.Other gets 100 orders, one water crystallization lactose 1.5kg, crosses 180 orders (80 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 55 degree, and temperature of charge is set to 40 degree.The material preheating begins hydrojet coating, 1.5 hours powder coating time after 10 minutes.Then regulate inlet temperature to 25 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 2.02kg, yield is 94.0%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC 35g
Magnesium stearate 15g
5000
Check result is as follows
Embodiment 4
Get 100 orders, one water crystallization lactose 0.65kg, add the deionized water of 1.44kg, and be heated to 80 ℃, stir and make dissolving.Then cool to 35 ℃.Other gets 100 orders, one water crystallization lactose 1.5kg, crosses 400 orders (38 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 55 degree, and temperature of charge is set to 40 degree.The material preheating begins hydrojet coating, 1.5 hours powder coating time after 10 minutes.Then regulate inlet temperature to 25 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 1.91kg, yield is 88.8%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC 35g
Magnesium stearate 15g
5000
Check result is as follows
Embodiment 5
Get 100 orders, one water crystallization lactose 0.75kg, add the deionized water of 3.75kg, and be heated to 80 ℃, stir and make dissolving.Then cool to 35 ℃.Other gets 100 orders, one water crystallization lactose 0.75kg, crosses 180 orders (80 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 55 degree, and temperature of charge is set to 40 degree.The material preheating begins hydrojet coating, powder coating time 2 h after 10 minutes.Then regulate inlet temperature to 25 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 1.37kg, yield is 91.3%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC 35g
Magnesium stearate 15g
5000
Check result is as follows
Embodiment 6
Get 100 orders, one water crystallization lactose 0.65kg, add the deionized water of 2.1kg, and be heated to 80 ℃, stir and make dissolving.Then cool to 35 ℃.Other gets 100 orders, one water crystallization lactose 1.5kg, crosses 180 orders (80 μ m) sieve after pulverizer is pulverized, and then puts in the fluid bed, opens fluid bed, and inlet temperature is set to 55 degree, and temperature of charge is set to 40 degree.The material preheating begins hydrojet coating, 1.5 hours powder coating time after 10 minutes.Then regulate inlet temperature to 25 ℃, air humidity is 40%, continues to make material boiling 30 minutes.Get finished product 1.97kg, yield is 91.6%.
Measure the angle of repose of this product, and mix rear direct compression by following prescription, check tablet weight variation, outward appearance and frangible degree.
Prescription:
Lactose 950g
HPMC 35g
Magnesium stearate 15g
5000
Check result is as follows
Comparative example
Spherical lactose and a commercially available water crystallization lactose of gained of the present invention are carried out Performance Ratio, and comparative result sees following table for details:
Annotate: Formulation is the heavy 200mg of sheet, lactose 190mg wherein, and hydroxypropyl emthylcellulose 7mg is as binding agent, and magnesium stearate 3mg is as lubricant.Above-mentioned 3 kinds of lactose mix rear direct compression respectively by the prescription batching.
By comparative test, we can draw following judgement:
Because a water crystallization lactose poor fluidity (angle of repose is large) almost can't effectively be filled in the press mold, so slice, thin piece can't molding.Can't satisfy the requirement of direct compression.
And lactose of the present invention, good fluidity can be used for direct compression, and the product tablet weight variation that suppresses, lustrous surface etc. all can meet the requirements.
Claims (8)
1. the production technology of a spherical lactose particle comprises the following steps:
Get a water crystallization lactose, grind to form the granule of 38～80 μ m particle size ranges, as base material, in every 100g water, dissolve the lactose aqueous solution of 20-45g one water crystallization lactose as coating solution again, use fluid bed to carry out granule coating, making spherical lactose particle, is 1～2.3:1 as the weight ratio of a water crystallization lactose of base material and a water crystallization lactose of preparation lactose solution.
2. the production technology of spherical lactose particle as claimed in claim 1, it is characterized in that, the preparation method of described lactose aqueous solution is: a water crystallization lactose of 20～45 weight portions is dissolved in 65～80 ℃ of deionized waters of 100 weight portions, is stirred to fully dissolving, then be cooled to 30～45 ℃.
3. the production technology of spherical lactose particle as claimed in claim 1 is characterized in that a described water crystallization lactose is a water crystallization alpha-lactose.
4. the production technology of spherical lactose particle is characterized in that as described in arbitrary such as claim 1-3, adopts spray mode in the end when described use fluid bed carries out granule coating, and the inlet temperature of fluid bed is 50～80 ℃; Temperature of charge is 35～60 ℃.
5. the production technology of spherical lactose particle as claimed in claim 4 is characterized in that, after the granule coating, continues to blow floating with 20～35 ℃ of air of dehumidifying, and relative air humidity is controlled at below 40%, and makes material under fluidized state, evaporates moisture content.
6. improve the lactose flowability to be applicable to the method for direct compression for one kind, for adopting the described production technology of the arbitrary claim of claim 1-5 one water crystallization lactose is processed into spherical lactose particle.
7. a lactose that is applicable to direct compression is spherical lactose particle, is made by the described production technology of the arbitrary claim of claim 1-5.
8. lactose is used for the purposes of tablet machine direct compression as claimed in claim 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010209359 CN102294033B (en) | 2010-06-25 | 2010-06-25 | Production process of spherical lactose particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010209359 CN102294033B (en) | 2010-06-25 | 2010-06-25 | Production process of spherical lactose particle |
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| Publication Number | Publication Date |
|---|---|
| CN102294033A CN102294033A (en) | 2011-12-28 |
| CN102294033B true CN102294033B (en) | 2013-02-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201010209359 Expired - Fee Related CN102294033B (en) | 2010-06-25 | 2010-06-25 | Production process of spherical lactose particle |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105766914A (en) * | 2016-04-08 | 2016-07-20 | 广西南宁益土生物科技有限责任公司 | Method for preventing and treating peanut bacterial wilt with lactose high-temperature processing product |
| CN111871326A (en) * | 2020-05-27 | 2020-11-03 | 常州道宁医药科技有限公司 | Device and method for preparing anhydrous lactose microcrystals by customizing alpha/beta ratio |
| CN111686083B (en) * | 2020-06-10 | 2022-04-22 | 石药集团中奇制药技术（石家庄）有限公司 | Ilaprazole enteric-coated tablet |
| CN112274485B (en) * | 2020-12-29 | 2021-04-20 | 江西中医药大学 | Three-dimensional porous lactose particle and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5792507A (en) * | 1996-01-24 | 1998-08-11 | Freund Industrial Co., Ltd. | Lactose spherical particles and process for their production |
-
2010
- 2010-06-25 CN CN 201010209359 patent/CN102294033B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5792507A (en) * | 1996-01-24 | 1998-08-11 | Freund Industrial Co., Ltd. | Lactose spherical particles and process for their production |
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Address after: 215200 comprehensive building of science and Technology Pioneer Park, Wujiang Economic Development Zone, Jiangsu Applicant after: Suzhou DDS Biotechnology Pharmaceutical Co., Ltd. Address before: 215200 comprehensive building of science and Technology Pioneer Park, Wujiang Economic Development Zone Applicant before: Wujiang Dixing Technology Co., Ltd. |
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Effective date of registration: 20180327 Address after: 257100 North No. 121, Dongying District, Dongying City, Shandong Province, 1 Co-patentee after: Shanghai Obsidian biological medicine technology Co., Ltd. Patentee after: Shandong Di Xing medicinal excipient Co., Ltd. Address before: 215200 comprehensive building of science and Technology Pioneer Park, Wujiang Economic Development Zone, Jiangsu Patentee before: Suzhou DDS Biotechnology Pharmaceutical Co., Ltd. |
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