CN106074422A - A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof - Google Patents
A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof Download PDFInfo
- Publication number
- CN106074422A CN106074422A CN201610596858.8A CN201610596858A CN106074422A CN 106074422 A CN106074422 A CN 106074422A CN 201610596858 A CN201610596858 A CN 201610596858A CN 106074422 A CN106074422 A CN 106074422A
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- lieting
- love song
- succinum love
- oral solid
- solid formulation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/495—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with two or more nitrogen atoms as the only ring heteroatoms, e.g. piperazine or tetrazines
- A61K31/505—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim
- A61K31/513—Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim having oxo groups directly attached to the heterocyclic ring, e.g. cytosine
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2095—Tabletting processes; Dosage units made by direct compression of powders or specially processed granules, by eliminating solvents, by melt-extrusion, by injection molding, by 3D printing
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
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Abstract
The invention discloses a kind of succinum love song Ge Lieting oral solid formulation, its composition includes: succinum love song Ge Lieting 120 145 parts, dilution filler 20 40 parts, disintegrating agent 4 10 parts, binding agent 45 parts, lubricant 56 parts, coating powder 5 11 parts.The invention also discloses this preparation method.It is an advantage of the current invention that preparing core point is dry method direct compression, it is not necessary to dry method rolling granulation or wet granulation or other granulation modes, technique is the simplest, it is simple to operation, and the end product quality simultaneously obtained is preferable, can be prevented effectively from crystal conversion.
Description
Technical field
The present invention relates to a kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof, be mainly used in oral medicine
The preparing technical field of agent.
Background technology
Trelagliptin (bent Ge Lieting) is a kind of weekly DPP IV (DPP-4) inhibitor, passes through
Selectivity, persistence suppression DPP-4, controls blood sugar level.DPP-4 is a kind of enzyme, it is possible to cause incretin (pancreas hyperglycemia
Element sample peptide-1 (GLP-1) and glucose-dependent-insulinotropic polypeptide (GIP)) inactivation, and these 2 kinds of intestinal drop insulins at blood glucose
Regulation plays an important role.Suppression DPP-4, by increasing capacitance it is possible to increase blood sugar level dependency insulin secretion, thus control blood glucose
Level.
For this medicine, it is that the more practical sexual valence of one compares that succinum love song Ge Lieting is prepared as oral solid preparation
High preparation scheme, the research and development to this technique are extremely necessary.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of succinum love song Ge Lieting oral solid formulation itself and preparation side
Method.
The present invention is achieved through the following technical solutions.
A kind of succinum love song Ge Lieting oral solid formulation, its composition includes: succinum love song Ge Lieting 120-145 part, dilute
Release filler 20-40 part, disintegrating agent 4-10 part, binding agent 4-5 part, lubricant 5-6 part, coating powder 5-11 part.
Further, dilution filler includes mannitol 13-23 part, microcrystalline Cellulose 7-17 part.
Further, disintegrating agent is cross-linking sodium carboxymethyl cellulose.
Further, binding agent is hydroxypropylcellulose.
Further, lubricant is sodium stearyl fumarate.
Further, the material grain of each composition is 100～200 mesh.
A kind of preparation method of succinum love song Ge Lieting oral solid formulation, step includes:
1) sieve after succinum love song Ge Lieting, filler, binding agent, disintegrating agent proportionally being mixed, it is thus achieved that first mixes
Close powder；
2) the first mixed powder is obtained the second mixed powder after mix lubricant, standby；
3) the second mixed powder is put into rotary tablet machine, be pressed into tablet；
4) tablet is coated；
5) packaging.
Beneficial effects of the present invention:
The core point of preparing of the present invention is dry method direct compression, it is not necessary to dry method rolling granulation or wet granulation or other systems
Grain mode, technique is the simplest, it is simple to operation, and the end product quality simultaneously obtained is preferable, can be prevented effectively from crystal conversion.
Detailed description of the invention
Below according to embodiment, the present invention is described in further detail.
Embodiment 1:
A kind of succinum love song Ge Lieting oral solid formulation, its composition includes: succinum love song Ge Lieting 120-145 part, dilute
Release filler 20-40 part, disintegrating agent 4-10 part, binding agent 4-5 part, lubricant 5-6 part, coating powder 5-11 part.
For concrete composition: dilution filler includes mannitol 13-23 part, microcrystalline Cellulose 7-17 part；Disintegrating agent is for handing over
Connection sodium carboxymethyl cellulose；Binding agent is hydroxypropylcellulose；Lubricant is sodium stearyl fumarate；The material grain of each composition is
100～200 mesh.
Embodiment 2:
A kind of succinum love song Ge Lieting oral solid formulation, its composition includes: succinum love song Ge Lieting 133mg, mannitol
18mg, microcrystalline Cellulose 12mg, cross-linking sodium carboxymethyl cellulose 7mg, hydroxypropylcellulose 4.4mg, sodium stearyl fumarate 5.6mg,
Coating powder 8mg.
Embodiment 3:
The preparation method of succinum love song Ge Lieting oral solid formulation, step includes:
1) sieve after succinum love song Ge Lieting, filler, binding agent, disintegrating agent proportionally being mixed, it is thus achieved that first mixes
Close powder；
2) the first mixed powder is obtained the second mixed powder after mix lubricant, standby；
3) the second mixed powder is put into rotary tablet machine, be pressed into tablet；
4) tablet is coated；
5) packaging.
Embodiment 4:
Medicine is identified:
[character] this product is Film coated tablets, removes whitening color after coating.
[discriminating] (1) takes this product fine powder, adds 50% methanol and makes every 1ml solution containing about 10 μ g song Ge Lieting, filters, takes
Subsequent filtrate, measures according to ultraviolet visible spectrophotometry (Chinese Pharmacopoeia four general rules 0401 of version in 2015), at 276nm wavelength
There is absorption maximum.
(2), under assay item in the chromatogram of record, the retention time of need testing solution main peak should be molten with reference substance
The retention time of liquid main peak is consistent.
[inspection] has related substance according to high performance liquid chromatography (Chinese Pharmacopoeia four general rules 0512 of version in 2015) test.
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler, with the phosphoric acid of 20mmol/mL
Potassium dihydrogen (phosphoric acid adjusts pH value 3.0) is mobile phase A, and acetonitrile is Mobile phase B, and flow velocity is 1.0ml per minute, and detection wavelength is
230nm, column temperature is 30 DEG C, and according to the form below carries out gradient elution.
Precision weighs succinum love song Ge Lietingyue 12.5mg, puts in 25ml measuring bottle, adds 1ml methanol, then adds 1ml 1mol/L
Sodium hydroxide solution, room temperature places 30min, adds 1ml1mol/LHCl solution and terminate destroying, add 1ml methanol, then with methanol-
Water (50:50) is settled to scale, shakes up,
As system suitability solution.Precision measures system suitability solution 20 μ l, injects chromatograph of liquid, records chromatograph
Figure.In chromatogram, the separating degree between each impurity and bent Ge Lieting peak should meet the requirements.
Algoscopy takes this product 5, finely ground, and precision weighs in right amount, dissolves with 50% methanol solution and dilutes and makes in every 1ml
Containing about the solution of 0.5mg song Ge Lieting, as need testing solution；Precision measures in right amount, makes every with 50% methanol solution dilution
Solution containing about 0.5 μ g in 1ml,
State Food and Drug Administration's drug evaluation center is evaluated
As contrast solution.Precision measures contrast solution 20 μ l, injects chromatograph of liquid, regulates detection sensitivity, makes main
The peak height of composition chromatographic peak is about the 20% of full scale；To measure 50% methanol solution, contrast solution, need testing solution each for precision again
20 μ l, are injected separately into chromatograph of liquid, record chromatogram.If any impurity peaks in the chromatogram of need testing solution, its peak area is not
Must more than the main peak area (0.1%) of contrast solution, each impurity peak area and cannot be greater than contrast solution main peak area 5 times
(0.5%).
Enantiomer is according to high performance liquid chromatography (Chinese Pharmacopoeia four general rules 0512 of version in 2015) test.With chirality color
Spectrum post (CHIRALPAK AD-H post) is fixing phase, with normal hexane-dehydrated alcohol (40:60) (containing 0.1% diethylamine) for flowing
Phase, flow velocity is 0.5ml per minute；Detection wavelength is 276nm.Take succinum love song Ge Lieting reference substance to compare with its enantiomer
Product are appropriate, accurately weighed, add anhydrous alcohol solution and dilution is made in every 1ml respectively containing succinum love song Ge Lieting 500 μ g, mapping
The solution of isomer 0.5 μ g, as system suitability solution.Precision measures system suitability solution 20 μ l, injects
Chromatograph of liquid, enantiomer and succinum love song Ge Lieting go out peak successively, and separating degree therebetween should be greater than 1.5.Take this
Product, finely ground, precision weighs in right amount, adds anhydrous alcohol solution and the solution containing about bent Ge Lieting 0.5mg is made in every 1ml in dilution,
Filter, take subsequent filtrate, as need testing solution；Precision measures in right amount, adds dehydrated alcohol dilution and makes every 1ml containing about 0.5 μ g's
Solution, as contrast solution；Precision measures comparison liquid 20 μ l and injects chromatograph of liquid, regulates detection sensitivity, makes main constituent color
The peak height of spectral peak is about the 10% of full scale；Precision measures need testing solution and each 20 μ l of contrast solution again, is injected separately into liquid phase
Chromatograph, 2 times of record chromatogram to main constituent peak retention time.In the chromatogram of need testing solution if any with enantiomer
The chromatographic peak that retention time is consistent, its peak area cannot be greater than 5 times (0.5%) of contrast solution main peak area.
Dissolution takes this product, according to dissolution method (Chinese Pharmacopoeia version four general rules 0,931 second method in 2015), with
The hydrochloric acid solution 900ml of 0.01mol/L is dissolution medium, and rotating speed is 75 turns per minute, operates in accordance with the law, takes solution through 15 minutes time
In right amount, filter, take subsequent filtrate appropriate, make in every 1ml the solution containing about bent Ge Lieting 16.5 μ g with dissolution medium dilution, as
Need testing solution；Separately take succinum love song Ge Lieting reference substance appropriate, accurately weighed, dissolve with dissolution medium and dilute and make often
Solution containing about bent Ge Lieting 15 μ g in 1ml, as reference substance solution.Take above two solution, according to spectrophotometry
Method (Chinese Pharmacopoeia four general rules 0401 of version in 2015), measures absorbance at the wavelength of 276nm, calculates the stripping quantity of every.
Limit is the 85% of labelled amount, should meet regulation.
Moisture takes this product fine powder, measures according to aquametry (Chinese Pharmacopoeia version four general rules 0,832 first method 1 in 2015).
Moisture content must not cross 5.0%.
[assay] is according to high performance liquid chromatography (Chinese Pharmacopoeia four general rules 0512 of version in 2015) test.
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler, with acetonitrile: methanol: 0.1%
Triethylamine (formic acid adjusts pH value to be 2.75) solution (12:3:85) is flowing phase, and column temperature is 35 DEG C, and detection wavelength is 276nm.Accurate
Measure and taken system suitability solution 20 μ l under related substance item, inject chromatograph of liquid, record chromatogram.Each impurity in chromatogram
And the separating degree between bent Ge Lieting peak should meet the requirements.
Algoscopy takes this product 5, finely ground, and precision weighs in right amount (being approximately equivalent to bent Ge Lieting 25mg), puts in 50ml measuring bottle,
Add water appropriate, concussion, shake up, filter, precision measures subsequent filtrate 2ml, puts in 50ml measuring bottle, and dilute with water is settled to scale, shakes
Even, as need testing solution, precision measures 20 μ l, injects chromatograph of liquid, records chromatogram；Separately take succinum love song Ge Lieting pair
Appropriate according to product, accurately weighed, make in every 1ml the solution containing about song Ge Lieting 20 μ g with water dissolution diluting, be measured in the same method.Press
External standard method, with calculated by peak area, to obtain final product.
Above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow and is familiar with this art
Personage will appreciate that present invention and is carried out, and can not limit the scope of the invention with this.All according to the present invention
The equivalence that spirit is made changes or modifies, and all should contain within the scope of the present invention.
Claims (7)
1. a succinum love song Ge Lieting oral solid formulation, it is characterised in that its composition includes: succinum love song Ge Lieting 120-
145 parts, dilution filler 20-40 part, disintegrating agent 4-10 part, binding agent 4-5 part, lubricant 5-6 part, coating powder 5-11 part.
Succinum love song Ge Lieting oral solid formulation the most according to claim 1, it is characterised in that dilution filler includes
Mannitol 13-23 part, microcrystalline Cellulose 7-17 part.
Succinum love song Ge Lieting oral solid formulation the most according to claim 1, it is characterised in that disintegrating agent is crosslinking carboxylic
Sodium carboxymethylcellulose pyce.
Succinum love song Ge Lieting oral solid formulation the most according to claim 1, it is characterised in that binding agent is that hydroxypropyl is fine
Dimension element.
Succinum love song Ge Lieting oral solid formulation the most according to claim 1, it is characterised in that lubricant is stearic rich
Horse acid sodium.
Succinum love song Ge Lieting oral solid formulation the most according to claim 1, it is characterised in that the material grain of each composition
It is 100～200 mesh.
7. a preparation method for the succinum love song Ge Lieting oral solid formulation as described in any one of claim 1-6, step
Including:
1) sieve after succinum love song Ge Lieting, filler, binding agent, disintegrating agent proportionally being mixed, it is thus achieved that the first mixed powder；
2) the first mixed powder is obtained the second mixed powder after mix lubricant, standby；
3) the second mixed powder is put into rotary tablet machine, be pressed into tablet；
4) tablet is coated；
5) packaging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610596858.8A CN106074422A (en) | 2016-07-27 | 2016-07-27 | A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610596858.8A CN106074422A (en) | 2016-07-27 | 2016-07-27 | A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106074422A true CN106074422A (en) | 2016-11-09 |
Family
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610596858.8A Pending CN106074422A (en) | 2016-07-27 | 2016-07-27 | A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106896166A (en) * | 2017-01-22 | 2017-06-27 | 合肥拓锐生物科技有限公司 | About the analysis method of material in a kind of amber love song Ge Lieting raw materials and its preparation |
| CN109839461A (en) * | 2019-03-14 | 2019-06-04 | 上海海虹实业(集团)巢湖今辰药业有限公司 | One koji Ge Lieting medicament contg detection method |
| CN110478327A (en) * | 2019-09-19 | 2019-11-22 | 苏州东瑞制药有限公司 | A kind of oral preparation and preparation method thereof containing amber love song Ge Lieting |
| CN114983958A (en) * | 2022-07-13 | 2022-09-02 | 青海夏都医药有限公司 | Trelagliptin succinate tablet and preparation method thereof |
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2016
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106896166A (en) * | 2017-01-22 | 2017-06-27 | 合肥拓锐生物科技有限公司 | About the analysis method of material in a kind of amber love song Ge Lieting raw materials and its preparation |
| CN106896166B (en) * | 2017-01-22 | 2019-08-09 | 合肥拓锐生物科技有限公司 | Analysis method in relation to substance in a kind of amber love song Ge Lieting raw material and its preparation |
| CN109839461A (en) * | 2019-03-14 | 2019-06-04 | 上海海虹实业(集团)巢湖今辰药业有限公司 | One koji Ge Lieting medicament contg detection method |
| CN110478327A (en) * | 2019-09-19 | 2019-11-22 | 苏州东瑞制药有限公司 | A kind of oral preparation and preparation method thereof containing amber love song Ge Lieting |
| CN114983958A (en) * | 2022-07-13 | 2022-09-02 | 青海夏都医药有限公司 | Trelagliptin succinate tablet and preparation method thereof |
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