CN105560197B - A kind of mitiglinide of Fast Stripping and its preparation and detection method - Google Patents
A kind of mitiglinide of Fast Stripping and its preparation and detection method Download PDFInfo
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- 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
- A61K31/40—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having five-membered rings with one nitrogen as the only ring hetero atom, e.g. sulpiride, succinimide, tolmetin, buflomedil
- A61K31/403—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having five-membered rings with one nitrogen as the only ring hetero atom, e.g. sulpiride, succinimide, tolmetin, buflomedil condensed with carbocyclic rings, e.g. carbazole
- A61K31/4035—Isoindoles, e.g. phthalimide
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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
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2013—Organic compounds, e.g. phospholipids, fats
- A61K9/2018—Sugars, or sugar alcohols, e.g. lactose, mannitol; Derivatives thereof, e.g. polysorbates
-
- 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
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2054—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
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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
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
-
- 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
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4841—Filling excipients; Inactive ingredients
- A61K9/4858—Organic compounds
-
- 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
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4841—Filling excipients; Inactive ingredients
- A61K9/4866—Organic macromolecular compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The present invention relates to medicine preparation field, feature be a kind of Fast Stripping mitiglinide and its preparation and detection method, said preparation composition it is as follows: 4-6 parts of Mitiglinide calcium raw material drug；25-45 parts of lactose；15-35 parts of microcrystalline cellulose, 15-35 parts of starch, hydroxypropyl methylcellulose E3 or 1.5-5.5 parts of hydroxypropyl methylcellulose E5；3-10 parts of sodium carboxymethyl starch；0.05-0.3 parts of magnesium stearate.The invention feature auxiliary material is easy to get, and at low cost, preparation method is simple, and manufactured finished product dissolution rate in vitro is fast, and 10min dissolution rate reaches 90% or more in multiple dissolution mediums, stable product quality.
Description
Technical field
The present invention relates to medicine preparation field, the mitiglinide of especially a kind of Fast Stripping and its preparation and inspection
Survey method.
Background technique
In recent years it finds, the damage of early phase insulin secreting ability is an important factor for diabetes B develops, therefore can be extensive
Multiple Postprandial insulin Early insulin secretion and the drug for reducing postprandial blood sugar become treatment diabetes B active drug.It is clinical at present to use
Mainly there are sulfonylurea (SU), biguanides, alpha-glucosidase restrainer, thiazolidine two in the oral medicine for the treatment of diabetes B
Ketone (TZD) and column how class etc..Wherein, sulfonylureas is other than treatment failure rate for the first time is higher, and there are about 10% patients
To the subsequent no response for the treatment of, main adverse reaction is hypoglycemia and increases weight seriously；Though biguanides exist
Have been used for treatment diabetes the end of the fifties, but apparent digestive tract side effects are restricted it in the application of certain patients；α-
The main adverse reaction of glucosidase inhibitor also appears in gastrointestinal side effect；Thiazolidinediones develop in recent years
Comparatively fast, but oedema and the worry of heart failure have seriously affected patient to the confidence of such drug.
Glinides are the new structural postprandial hypoglycemic agents of oral fast-acting type.Mitiglinide is in 1992 by Sato
F et al. synthesis, is the 3rd novel benzoic acid derivative class antidiabetic drug after Repaglinide, Nateglinide.Clinical test table
Bright, Mitiglinide is to be superior to other antidiabetic drugs in terms of efficacy and saferry so far, is that novel quick-acting rush pancreas islet are thin
" blood sugar regulator used during user having meals " of intracrine insulin.It for treating diabetes B, needs rapid-action, can quickly reduce postprandial
Blood glucose.
Summary of the invention
It is a primary object of the present invention to improve product quality, mitiglinide dissolution rate is improved, reaches quick
Dissolve out purpose；Satisfactory quality between guarantee product storage period, provides the mitiglinide and its system of a kind of Fast Stripping
Standby and detection method.
A kind of mitiglinide of Fast Stripping, the preparation include following components by weight:
4-6 parts of Mitiglinide calcium raw material drug；25-45 parts of lactose；15-35 parts of microcrystalline cellulose, 15-35 parts of starch, hydroxypropyl
Methylcellulose E3 or 1.5-5.5 parts of hydroxypropyl methylcellulose E5；3-10 parts of sodium carboxymethyl starch；0.05-0.3 parts of magnesium stearate.
The preparation includes following components by weight:
4.5-5.3 parts of Mitiglinide calcium raw material drug；30-40 parts of lactose；20-30 parts of microcrystalline cellulose, 20-30 parts of starch,
Hydroxypropyl methylcellulose E3 or 2-5 parts of hydroxypropyl methylcellulose E5；4-5 parts of sodium carboxymethyl starch；0.1-0.2 parts of magnesium stearate.
The Mitiglinide calcium raw material drug partial size D (0.5)≤10 μm, D (0.9)≤40 μm.
It the described method comprises the following steps:
1) Mitiglinide Calcium and lactose mixing, obtain material 1；
2) microcrystalline cellulose, starch are added in material 1,30%-40% sodium carboxymethyl starch is uniformly mixed, obtains material
2；
3) hydroxypropyl methylcellulose E3 or E5 are configured to the aqueous solution of 1%-10% concentration, material 2 is added thereto, is pelletized
Obtain material 3；
4) material 3 it is dry material 4；
5) material 4 is crossed into the aperture 1.0-2.0mm sieve whole grain, 60%-70% sodium carboxymethyl starch, tristearin is added after whole grain
Sour magnesium is uniformly mixed, obtains material 5；
6) by 5 tabletting of material or filling capsule；
Complete the production of mitiglinide.
Step 1) the incorporation time is 5-15min.
Step 2) the mixing condition is that 50-150rpm/min mixing speed mixes 3-8min.
Step 4) drying temperature≤70 DEG C.
It further include the dissolution detection method to Mitiglinide calcium tablet are as follows: Mitiglinide calcium tablet is taken, referring to Chinese Pharmacopoeia
2015 editions four general rules, 0,931 second method dissolution method-slurry processes, with water, pH=1.2 hydrochloride buffer, pH=4.5 acetic acid
Salt buffer, for pH=6.8 phosphate buffer respectively as dissolution medium, revolving speed is 50 turns per minute, when through 10 minutes, is taken continuous
Filtrate is as test solution；It is appropriate that another precision weighs Mitiglinide Calcium standard items, adds methanol appropriate, shaking makes to dissolve, and adds
The solution of the 5.6 μ g containing Mitiglinide Calcium in every 1ml is made as standard solution, with octadecylsilane key in dissolution medium dilution
Conjunction silica gel is filler, and with 0.025mol/L potassium dihydrogen phosphate: acetonitrile=55: 45 be mobile phase, the 0.025mol/L phosphoric acid
Potassium dihydrogen is used with phosphoric acid tune pH as 3.0, and Detection wavelength 210nm, number of theoretical plate should be not less than based on Mitiglinide Calcium peak
2000 chromatographic conditions take test solution and each 20 μ l of standard solution, are injected separately into liquid chromatograph, record chromatogram, press
External standard method goes out every the amount of dissolution with calculated by peak area, and limit is the 90% of labelled amount.
Mitiglinide calcium capsule is taken, referring to 2015 editions four general rules of Chinese Pharmacopoeia, 0,931 first method dissolution method-indigo plant
Method, with water, pH=1.2 hydrochloride buffer, pH=4.5 acetate buffer, pH=6.8 phosphate buffer is respectively as dissolution
Medium, revolving speed are 50 turns per minute, when through 10 minutes, take subsequent filtrate as test solution；Another precision weighs Mitiglinide Calcium
Appropriate standard items add methanol appropriate, and shaking makes to dissolve, and solubilization goes out medium and the 5.6 μ g containing Mitiglinide Calcium in every 1ml is made
Solution as standard solution, be filler with octadecylsilane chemically bonded silica, with 0.025mol/L potassium dihydrogen phosphate: second
Nitrile=55: 45 be mobile phase, and the 0.025mol/L potassium dihydrogen phosphate is used with phosphoric acid tune pH as 3.0, and Detection wavelength is
210nm, number of theoretical plate should be not less than 2000 chromatographic conditions based on Mitiglinide Calcium peak, take test solution and standard solution each
20 μ l, are injected separately into liquid chromatograph, record chromatogram, and every the amount of dissolution is gone out with calculated by peak area by external standard method, and limit is
The 90% of labelled amount.
The present invention provides the mitiglinide and its preparation and detection method of a kind of Fast Stripping, and beneficial effect is such as
Under:
1, production process of the present invention is closed, and preparation process is simple, is not likely to produce dust, and medicinal powder is avoided to cause producers
Adverse effect, production process are high-efficient；
2, Mitiglinide calcium raw material drug is mixed before premix with lactose, improve the mixing uniformity of total mix particle and improves rice
Ge Lienai calcium preparation dissolution rate；
3, the present invention by control Mitiglinide calcium raw material drug partial size and prescription proportion, produce Mitiglinide calcium tablet or
Capsule can be in water, pH=1.2 hydrochloride buffer, pH=4.5 acetate buffer, in pH=6.8 phosphate-buffered liquid medium
10min dissolution rate reaches 90% or more；
4, unknown list is miscellaneous in 2 year validity period of related substance in the mitiglinide that the present invention makes is no more than
0.08%, it is always miscellaneous to be no more than 0.32%；
5, present invention optimizes the mixing speed of preparation manufacturing process mixing and time, mixing speed and time are to meter Ge Lie
How calcium preparation premix mixing uniformity has a significant impact: rotating speed of agitator is too low, and mixing efficiency is low, and material is unable to fully mix；
Revolving speed is excessively high, and Mitiglinide Calcium can swim in wet granulator surface, also influences product material mixing uniformity；
6, granulation conditions are suitable in formulation method of the invention, and grains good moldability obtained, uniform properties avoid
Granulation time and speed of agitator are too low, and wet granular does not stir uniform, and Granulation time and agitating paddle are excessively high, and material fever will produce
Raw foreign matter point, influences product characteristics.
Detailed description of the invention
Fig. 1: the Multidirectional motion total mix bucket sample point location drawing.
Specific embodiment
A kind of Mitiglinide calcium tablet of the Fast Stripping of embodiment 1
5 parts of Mitiglinide Calcium；40 parts of lactose；30 parts of microcrystalline cellulose；20 parts of starch；E55 parts of hydroxypropyl methylcellulose；Carboxylic first
5 parts of base starch；0.1 part of magnesium stearate.
The Mitiglinide calcium raw material drug partial size D (0.5)≤10 μm, D (0.9)≤40 μm.
The method for preparing mitiglinide described in right, the described method comprises the following steps:
1) Mitiglinide Calcium and lactose mixing 10min, obtain material 1；
2) material 1 puts into wet mixing pelletizer together with lactose, microcrystalline cellulose, starch, 30% sodium carboxymethyl starch
In, 120rpm/min mixing speed mixes 8min, obtains material 2；
3) hydroxypropyl methylcellulose E3 or E5 are configured to the aqueous solution of 1%-10% concentration, material 2 is added thereto, is pelletized
Material 3 is obtained, granulation conditions are mixing speed 100rpm/min, cutting speed 1500rpm/min, and pelletize 4min；
4) it under the conditions of temperature of charge is no more than 65 DEG C, using fluidized bed drying, controls between moisture 1%-4%, stops
It is dry, obtain material 4；
5) additional 70% sodium carboxymethyl starch is added in the particle crushing and pelletizing machine aperture 2.0mm sieve whole grain after drying
And magnesium stearate, 5min is mixed, material 5 is obtained；
6) by 5 tabletting of material.
Complete the production of Mitiglinide Calcium calcium tablet.
A kind of Mitiglinide calcium capsule of the Fast Stripping of embodiment 2
A kind of mitiglinide, which is characterized in that the preparation includes following components by weight:
5 parts of Mitiglinide Calcium；30 parts of lactose；20 parts of microcrystalline cellulose；30 parts of starch；It is interior to add 1.5 parts of sodium carboxymethyl starch；
E32 parts of hydroxypropyl methylcellulose；4 parts of additional sodium carboxymethyl starch；0.1 part of magnesium stearate.
The Mitiglinide calcium raw material drug partial size D (0.5)≤10 μm, D (0.9)≤40 μm.
The method for preparing mitiglinide described in right, the described method comprises the following steps:
1) Mitiglinide Calcium and lactose mixing 5min, obtain material 1；
2) material 1 puts into wet mixing pelletizer together with lactose, microcrystalline cellulose, starch, 40% sodium carboxymethyl starch
In, 100rpm/min mixing speed mixes 5min, obtains material 2；
3) hydroxypropyl methylcellulose E3 or E5 are configured to the aqueous solution of 1%-10% concentration, material 2 is added thereto, is pelletized
Material 3 is obtained, granulation conditions are mixing speed 100rpm/min, cutting speed 1500rpm/min, and pelletize 4min；
4) it under the conditions of 3 temperature of material is no more than 60 DEG C, using fluidized bed drying, controls between moisture 1%-4%, stops
It is dry, obtain material 4；
5) additional 60% sodium carboxymethyl starch is added in the particle crushing and pelletizing machine aperture 2.0mm sieve whole grain after drying
And magnesium stearate, 5min is mixed, material 5 is obtained；
6) 5 capsule charge of material is controlled content uniformity theory loading amount ± 7% by capsule filling machine；
Complete the production of Mitiglinide calcium capsule.
Embodiment 3, different grain size Mitiglinide calcium raw material drug prepare the influence of Mitiglinide Calcium tablet dissolution
Using the method for the present invention, other raw material proportionings are consistent with method, compare different material partial size to Mitiglinide calcium tablet
The influence of dissolution rate, concrete outcome are shown in Table 1 (slurry processes, 50rpm, 900ml, n=6).
1 different grain size Mitiglinide calcium raw material drug of table prepares the influence of Mitiglinide Calcium tablet dissolution
As shown in Table 1, influence of the Mitiglinide Calcium raw material particle size to Mitiglinide Calcium tablet dissolution is significant, Mitiglinide Calcium
Raw material particle size D (0.5)≤10 μm, in D (0.9)≤40 μ m, the dissolution rate of Mitiglinide calcium tablet 10min can reach 90% with
On.
The comparison of the Mitiglinide preparation dissolution rate of the present invention of embodiment 4
The Mitiglinide preparation dissolution rate for comparing Mitiglinide preparation and different manufacturers of the present invention, the results are shown in Table 2.
2 different manufacturers mitiglinide dissolution rate of table compares
As shown in Table 1, mitiglinide dissolution rate of the present invention is substantially better than other producers.
The Mitiglinide calcium raw material drug of the present invention of embodiment 5 and influence of the lactose incorporation time to dissolution rate
Influence result of the Mitiglinide calcium raw material drug of the present invention with lactose incorporation time to Mitiglinide Calcium tablet dissolution is shown in
Table 3 (slurry processes, 50rpm, 900ml, n=6).
3 Mitiglinide calcium raw material drug of table and influence of the lactose incorporation time to dissolution rate
As shown in Table 3, Mitiglinide Calcium can reach with lactose mixing 5-15min, Mitiglinide calcium tablet 10min dissolution rate
90% or more, and incorporation time is too long, will affect production efficiency.
6 hybrid mode of embodiment influences total mix particle mixing uniformity
Hybrid mode is shown in Table 4,5 to the influence of total mix particle mixing uniformity, multinomial movement mixer sampling figure (1/2/3/4/
5/6 represents total mix bucket different location) see attached drawing 1.
Total mix granule content testing result after 4 Mitiglinide calcium raw material drug of table is directly mixed with auxiliary material
After 5 Mitiglinide calcium raw material drug of table is first mixed with lactose, then total mix granule content testing result after being mixed with auxiliary material
By table 4, known to table 5 as a result, total mix granule content can be significantly improved after Mitiglinide Calcium first mixed with lactose
Uniformity, different sample point granule content RSD are significantly reduced.
The mitiglinide stability of the present invention of embodiment 7
Invention mitiglinide stability is detected, invention formulation finished product uses the medicinal stiff sheet/aluminium foil of PVC
Packaging carries out long-term stable experiment, detects related substance, storage requirement are as follows: and 25 DEG C ± 2 DEG C of temperature, humidity 60% ±
5%, it the results are shown in Table 6.
The mitiglinide stability of the present invention of table 6
After product is stored 24 months as shown in Table 6, it is known that single miscellaneous, unknown list is miscellaneous and total miscellaneous meets existing Mitiglinide Calcium
In tablet quality standard and it is substantially less than to the requirement in relation to substance.
8 temperature of charge of embodiment influences drying efficiency and product quality
7 drying temperature of table influences result to drying efficiency and product quality
As shown in Table 7, as drying temperature increases, drying time is obviously shortened, after drying temperature is more than 70 DEG C, finished product
Total miscellaneous increase is obvious, and combustion has flavescence risk.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this Shen
Please in embodiment and embodiment in feature in the absence of conflict, can mutual any combination.Protection model of the invention
The technical solution that should be recorded with claim is enclosed, the equivalent replacement side of technical characteristic in the technical solution recorded including claim
Case is protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.
Claims (4)
1. a kind of mitiglinide of Fast Stripping, which is characterized in that the preparation includes by weight with the following group
Point:
4-6 parts of Mitiglinide calcium raw material drug；25-45 parts of lactose；15-35 parts of microcrystalline cellulose, 15-35 parts of starch, hydroxypropyl first is fine
Tie up element E3 or 1.5-5.5 parts of hydroxypropyl methylcellulose E5；3-10 parts of sodium carboxymethyl starch；0.05-0.3 parts of magnesium stearate；
Prepare the method for the mitiglinide of the Fast Stripping the following steps are included:
1) Mitiglinide Calcium and lactose mixing, obtain material 1；
2) microcrystalline cellulose, starch are added in material 1,30%-40% sodium carboxymethyl starch is uniformly mixed, obtains material 2；
3) hydroxypropyl methylcellulose E3 or E5 are configured to the aqueous solution of 1%-10% concentration, material 2 is added thereto, granulation obtains object
Material 3；
4) material 3 it is dry material 4；
5) material 4 is crossed into the aperture 1.0-2.0mm sieve whole grain, 60%-70% sodium carboxymethyl starch, magnesium stearate is added after whole grain,
It is uniformly mixed, obtains material 5；
6) by 5 tabletting of material or filling capsule；
Complete the production of mitiglinide；
The Mitiglinide calcium raw material drug partial size D(0.5)≤10 μm, D(0.9)≤40 μm；
The step 1) incorporation time is 5-15min；
The step 2 mixing condition is that 50-150rpm mixing speed mixes 3-8min；
The step 3) granulation conditions are mixing speed 50-150rpm, cutting speed 1500rpm, time 2-6min；
Step 4) drying temperature≤70 DEG C.
2. the mitiglinide of Fast Stripping according to claim 1, which is characterized in that the preparation includes by weight
The following components of part meter:
4.5-5.3 parts of Mitiglinide calcium raw material drug；30-40 parts of lactose；20-30 parts of microcrystalline cellulose, 20-30 parts of starch, hydroxypropyl
Methylcellulose E3 or 2-5 parts of hydroxypropyl methylcellulose E5；4-5 parts of sodium carboxymethyl starch；0.1-0.2 parts of magnesium stearate.
3. the mitiglinide of Fast Stripping according to claim 1, which is characterized in that further include to Mitiglinide
The dissolution detection method of calcium tablet are as follows: Mitiglinide calcium tablet is taken, it is molten referring to 2015 editions four general rules, 0,931 second methods of Chinese Pharmacopoeia
Out-degree measuring method-slurry processes, with water, the hydrochloride buffer of pH=1.2, the acetate buffer of pH=4.5, the phosphate buffer of pH=6.8 point
Not Zuo Wei dissolution medium, revolving speed be 50 turns per minute, when through 10 minutes, take subsequent filtrate as test solution；Another precision weighs
Mitiglinide Calcium standard items are appropriate, add 2 mL of methanol, shaking makes to dissolve, and solubilization goes out medium and lattice containing rice in every 1ml are made
How the solution of 5.6 μ g of calcium is filler with octadecylsilane chemically bonded silica, with 0.025mol/L phosphorus as standard solution to column
Acid dihydride potassium: acetonitrile=55: 45 be mobile phase, and the 0.025mol/L potassium dihydrogen phosphate uses phosphoric acid tune pH for 3.0, detects wave
A length of 210nm, number of theoretical plate should be not less than 2000 chromatographic conditions based on Mitiglinide Calcium peak, take test solution and standard items molten
Each 20 μ l of liquid, is injected separately into liquid chromatograph, records chromatogram, and every the amount of dissolution, limit are gone out with calculated by peak area by external standard method
Degree is the 90% of labelled amount.
4. the mitiglinide of Fast Stripping according to claim 1, which is characterized in that further include to Mitiglinide
The dissolution detection method of calcium capsule are as follows: Mitiglinide calcium capsule is taken, referring to 2015 editions four general rules 0,931 first of Chinese Pharmacopoeia
Method dissolution method-basket method, with water, the hydrochloride buffer of pH=1.2, the acetate buffer of pH=4.5, the phosphate-buffered of pH=6.8
For liquid respectively as dissolution medium, revolving speed is 50 turns per minute, when through 10 minutes, takes subsequent filtrate as test solution；It is another accurate
It is appropriate to weigh Mitiglinide Calcium standard items, adds 2 mL of methanol, shaking makes to dissolve, and solubilization goes out medium and be made in every 1ml to contain
The solution of 5.6 μ g of Mitiglinide Calcium is filler with octadecylsilane chemically bonded silica as standard solution, with
0.025mol/L potassium dihydrogen phosphate: acetonitrile=55: 45 be mobile phase, and the 0.025mol/L potassium dihydrogen phosphate uses phosphoric acid tune pH
It is 3.0, Detection wavelength 210nm, number of theoretical plate should be not less than 2000 chromatographic conditions based on Mitiglinide Calcium peak, take test sample molten
Liquid and each 20 μ l of standard solution are injected separately into liquid chromatograph, record chromatogram, go out every by external standard method with calculated by peak area
The amount of dissolution, limit be labelled amount 90%.
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