CN100582771C - Chinese medicinal soft capsule effective ingredient detection method - Google Patents
Chinese medicinal soft capsule effective ingredient detection method Download PDFInfo
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- CN100582771C CN100582771C CN200510200164A CN200510200164A CN100582771C CN 100582771 C CN100582771 C CN 100582771C CN 200510200164 A CN200510200164 A CN 200510200164A CN 200510200164 A CN200510200164 A CN 200510200164A CN 100582771 C CN100582771 C CN 100582771C
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Abstract
The present invention discloses Jinshuibao soft capsule prepared with fermented aweto powder as main medicine component and containing diluent and softening agent. The soft capsule has relatively high stability. In addition, the preparation process and its quality control method is also disclosed.
Description
Technical field
The medicine that the invention discloses a kind of Chinese medicinal soft capsule is formed, and the medicine that especially discloses the Jinshuibao soft capsule a kind of is formed, and belongs to the field of Chinese medicines.Simultaneously, the invention also discloses this preparation of soft capsule method and effective constituent detection method.
Background technology
Fermentation cordyceps is to separate the asexual generation-Synnematum sinense Yin et Shen sp. Now strain of the section ergot fungus cordyceps sinensis that obtains through the mycelial dried powder of liquid fermentation and culture gained from the fresh Cordyceps sinensis in Qinghai, effect with tonifying lung kidney, beneficial vital essence can be used for the supplemental treatment of diseases such as cough that deficiency of both the lung and kidney causes, asthma, spitting of blood, aching pain in waist and back and chronic bronchitis.Clinically be made into multiple formulation, comprise tablet, capsule, oral liquid, as the Jinshuibao sheet.These medicines have been brought into play bigger effect in the application of treatment deficiency of both the lung and kidney disease.
But because of the characteristic of cordyceps, that existing preparation all exists is easily mouldy, the moisture absorption, rotten shortcoming, needs a kind of better dosage form to replace; On the other hand, soft capsule has good leak tightness, dispersion of medicine, cover bad smell, advantage such as be easy to preserve and carry, and just becoming the emerging formulation of the field of Chinese medicines, and it represents the new developing direction of Chinese patent drug.Thereby if the cordyceps preparation can be made soft capsule, will be great progress.Because the prescriptions of traditional Chinese medicine complexity, the Chinese medicinal soft capsule formulation method does not have unified standard, and each medicine all will systematically be studied, fermentation cordyceps is no exception, so far find no the document that is made into soft capsule, reach this purpose, must pay work.
Summary of the invention
The technological difficulties of soft capsule are mainly in the preparation of capsule liquid, and general capsule liquid is made up of medicine, thinning agent and softening agent, and in order to determine its ratio, the inventor studies.
One, the selection of thinning agent: the selection of pharmaceutical diluents is one of key of development soft capsule, and it should be able to guarantee the accuracy and the stability of formulation of content, thereby guarantees the safety and effectiveness of medicine.Thinning agent at present commonly used has vegetable oil and polyglycol-400 (PEG-400), the inventor by experiment to above the two screen.
Get two parts of fermentation cordyceps, add the vegetable oil and the polyglycol-400 of capacity respectively, fully mix after colloid mill ground 20 minutes, put in 3000 rev/mins the hydro-extractor centrifugal 30 minutes, the precipitation situation of observing two mixed liquors the results are shown in following table
The different thinning agent sedimentation of table 1 situation test findings
| Thinning agent | The sedimentation situation |
| Vegetable oil | Sedimentation fully, vegetable oil and medicinal powder layering are obvious |
| Polyglycol-400 | Precipitation does not appear, polyglycol-400 and not layering of medicinal powder |
By table 1 result as can be known, be the content good stability of thinning agent gained with polyglycol-400, be difficult for layering and separate out, be thinning agent so determine to select for use polyglycol-400.
Two, the selection of diluent ratio: the consumption of thinning agent directly has influence on the loading amount and the content uniformity of soft capsule.Diluent ratio is low excessively, and then soup is mobile bad, and content uniformity is bigger.Diluent ratio is excessive, and drug dose increases, the inconvenience of taking medicine.Therefore screen the thinning agent of different proportion, thereby determined optimal proportion.Get three parts of medicinal powder that mix, add the polyglycol-400 of different amounts respectively, fully mix, observe its state, the results are shown in following table after colloid mill ground 20 minutes.
The selection test findings of table 2 diluent ratio
| Thinning agent: medicinal powder | The soup situation |
| 1∶1 | The soup thickness, mobile bad |
| 3∶2 | Soup is even, and is better mobile |
| 2∶1 | Soup is rarer, good fluidity |
By result in the table as can be known, when the ratio of thinning agent and medicinal powder was 3: 2, the flowability of soup can satisfy the requirement of soft capsule pressing, so determine that the ratio of thinning agent and Chinese caterpillar fungus fermentation bacterium powder is 3: 2.
Three, the selection of softening agent: in the process of preparation sample, find, the softgel shell hardening after placement a period of time (about 10 days) of soft capsule finished product through washing ball, drying, the disintegration time limited of soft capsule is elongated, the inventor thinks after the characteristic of each material by analysis: the PEG-400 in the capsule liquid can absorb the moisture in the softgel shell, so cause the softgel shell hardening, the disintegration time limited of soft capsule is elongated, change this situation, should add an amount of softening agent and suppress the moisture that capsule liquid absorbs softgel shell in capsule liquid.Afterwards, the inventor found that propylene glycol had the effect of moisture between balance softgel shell capsule liquid, so its ratio is studied.When preparing sample again, substitute part polyglycol-400 with accounting for a certain proportion of propylene glycol of total medication amount, made sample is observed its variation placing a period of time (T=14～20 ℃, RH=40%～60%) back, and experimental result sees the following form.
The different prescription of table 3 capsule liquid is to EFFECT OF CORK STOPPER
As can be seen from the above table, after the propylene glycol ratio reaches 8%, reached requirement disintegration time limited.So determine in the prescription of soft capsule, should add the propylene glycol of total medication amount 8%, prolong to prevent soft capsule hardening and disintegration time limited.
Four, preparation process: according to the research contents in early stage, Jinshuibao preparation of soft capsule process has finally been formulated in invention.That is: get fermentation cordyceps, add propylene glycol in proportion and add polyglycol-400, mix, be pressed into soft capsule.Its mixed process can be ground with colloid mill, so that soup reaches uniform and smooth.
Five, effective constituent detection method: in order effectively to control product quality, the inventor has also formulated quality standard, and this standard comprises qualitative identification and assay two parts, and following content is arranged.
Differentiate: (1) gets adenine reference substance and adenosine reference substance, adds Diluted Alcohol and makes the solution that every 1ml contains 10ug respectively, in contrast product solution.Test according to high performance liquid chromatography, with octadecylsilane chemically bonded silica is filling agent, phosphate buffer solution [0.066mol/L potassium dihydrogen phosphate-0.066mol/L disodium phosphate soln (4: 6)] with 0.5% tetrahydrofuran is a moving phase, the detection wavelength is 260nm, draw [assay] item need testing solution and each 20ul of above-mentioned reference substance solution down, inject high performance liquid chromatograph, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, corresponding chromatographic peak is arranged.
(2) get this product content 5g, put in the 10ml centrifuge tube, in 12000 rev/mins hydro-extractor centrifugal 30 minutes, discard upper strata liquid, precipitation adds water 10ml, is heated to and boils, and filters, and gets subsequent filtrate as need testing solution.Other gets the alanine reference substance, adds water and makes the solution that every 1ml contains alanine 1mg, in contrast product solution.Test according to thin-layered chromatography, draw need testing solution 3ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal butyl alcohol-glacial acetic acid-water (4: 1: 1), launch, take out, dry, spray is with ninhydrin solution, and it is clear to be heated to spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) get the sweet mellow wine reference substance, add Diluted Alcohol and make the solution that every 1ml contains 9mg, in contrast product solution.Test according to thin-layered chromatography, draw need testing solution and each 2ul of above-mentioned reference substance solution under the item of [discriminating] (2), put respectively on same silica gel g thin-layer plate, with isopropyl alcohol-ethyl acetate-water (9: 6: 2) is developping agent, launch, take out, dry, spray is with 2% liquor potassic permanganate, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the relevant position of reference substance chromatogram on, show the spot of same color.
Assay: according to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; Phosphate buffer solution [0.066mol/L potassium dihydrogen phosphate-0.066mol/L disodium phosphate soln (4: 6)] with 2% tetrahydrofuran is a moving phase; The detection wavelength is 260nm, and number of theoretical plate is pressed the adenosine peak and calculated, and should be not less than 3000.
The preparation of the reference substance solution 105 ℃ of drying under reduced pressure of learning from else's experience are an amount of to the adenosine reference substance of constant weight, accurately claim surely, add Diluted Alcohol and make the solution that every 1ml contains 40ug, and precision pipettes 2ml, puts in the 10ml measuring bottle, adds moving phase to scale, shakes up, promptly.
The content under the content uniformity item is got in the preparation of need testing solution, and mixing is got 2.5g, and accurate the title decides, put in the ground triangular flask, precision adds Diluted Alcohol 50ml, claims to decide weight, sonicated (power 250W, frequency 40KHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision pipettes subsequent filtrate 2ml, puts in the 10ml measuring bottle, adds moving phase to scale, shake up, filter with miillpore filter (0.45um), promptly.
Accurate respectively reference substance solution and each 20 Ma of need testing solution drawn of determination method inject high performance liquid chromatograph, measure, promptly.
Beneficial effect
This bright Jinshuibao soft capsule is adopted medicinal aluminium-plastic bubble plate packing.With room temperature reserved sample observing method sample is observed: (T=14～20 ℃, RH=40%～60%) at ambient temperature, carry out continuous six months study on the stability at the appointed time.The investigation index is: proterties, identification check, assay, microbial limit, and test method is by method of quality control of the present invention; Limit test of microbe is by " Chinese pharmacopoeia appendix XIII C limit test of microbe method operation in 2000.The results are shown in following table.
Table 4 Jinshuibao soft capsule stability experiment result
The result meets the regulation of the current domestic drug standards.The present invention has reached purpose.
Embodiment
Embodiment 1:
Prescription: fermentation cordyceps 1.8kg, polyglycol-4002.4kg, propylene glycol 0.35kg
Method for making: get fermentation cordyceps, add propylene glycol and polyglycol-400, cross colloid mill and ground 20 minutes, on encapsulating machine, be pressed into soft capsule.
Embodiment 2:
Prescription: fermentation cordyceps 2.2kg, polyglycol-4002.8kg, propylene glycol 0.45kg, ethylparaben 0.1kg
Method for making: get fermentation cordyceps, add propylene glycol, polyglycol-400 and ethylparaben, cross colloid mill and ground 20 minutes, on encapsulating machine, be pressed into soft capsule.
Embodiment 3:
Prescription: fermentation cordyceps 2kg, polyglycol-4002.6kg, propylene glycol 0.4kg
Method for making: get fermentation cordyceps, add propylene glycol and polyglycol-400, mix, make 10000 of soft capsules
Quality standard:
Adenine reference substance and adenosine reference substance are got in discriminating (1), add Diluted Alcohol and make the solution that every 1ml contains 10ug respectively, in contrast product solution.Test according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000), with octadecylsilane chemically bonded silica is filling agent, phosphate buffer solution [0.066mol/L potassium dihydrogen phosphate-0.066mol/L disodium phosphate soln (4: 6)] with 0.5% tetrahydrofuran is a moving phase, the detection wavelength is 260nm, draw [assay] item need testing solution and each 20ul of above-mentioned reference substance solution down, inject high performance liquid chromatograph, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, corresponding chromatographic peak is arranged.
(2) get this product content 5g, put in the 10ml centrifuge tube, in 12000 rev/mins hydro-extractor centrifugal 30 minutes, discard upper strata liquid, precipitation adds water 10ml, is heated to and boils, and filters, and gets subsequent filtrate as need testing solution.Other gets the alanine reference substance, adds water and makes the solution that every 1ml contains alanine 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw need testing solution 3ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal butyl alcohol-glacial acetic acid-water (4: 1: 1), launch, take out, dry, spray is with ninhydrin solution, and it is clear to be heated to spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) get the sweet mellow wine reference substance, add Diluted Alcohol and make the solution that every 1ml contains 9mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw need testing solution and each 2ul of above-mentioned reference substance solution under " differentiating (2) " item, put respectively on same silica gel g thin-layer plate, with isopropyl alcohol-ethyl acetate-water (9: 6: 2) is developping agent, launch, take out, dry, spray is with 2% liquor potassic permanganate, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the relevant position of reference substance chromatogram on, show the spot of same color.
Assay is measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; Phosphate buffer solution [0.066mol/L potassium dihydrogen phosphate-0.066mol/L disodium phosphate soln (4: 6)] with 2% tetrahydrofuran is a moving phase; The detection wavelength is 260nm, and number of theoretical plate is pressed the adenosine peak and calculated, and should be not less than 3000.
The preparation of the reference substance solution 105 ℃ of drying under reduced pressure of learning from else's experience are an amount of to the adenosine reference substance of constant weight, accurately claim surely, add Diluted Alcohol and make the solution that every 1ml contains 40ug, and precision pipettes 2ml, puts in the 10ml measuring bottle, adds moving phase to scale, shakes up, promptly.
The content under the content uniformity item is got in the preparation of need testing solution, and mixing is got 2.5g, and accurate the title decides, put in the ground triangular flask, precision adds Diluted Alcohol 50ml, claims to decide weight, sonicated (power 250W, frequency 40KHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision pipettes subsequent filtrate 2ml, puts in the 10ml measuring bottle, adds moving phase to scale, shake up, filter with miillpore filter (0.45um), promptly.
Accurate respectively reference substance solution and each 20 Ma of need testing solution drawn of determination method inject high performance liquid chromatograph, measure, promptly.
Every of this product contains adenosine (C
10H
13N
50
4) should be 0.36～0.60mg.
Claims (2)
1, a kind of effective constituent detection method of Chinese medicinal soft capsule, wherein contain a certain proportion of fermentation cordyceps, polyglycol and propylene glycol in the capsule liquid of Chinese medicinal soft capsule, three's weight ratio is: 180～220 parts of fermentation cordyceps, 240～280 parts of polyglycol, 35～45 parts of propylene glycol; It is characterized in that this method comprises following discrimination method:
A. get capsule liquid 2.5g, the accurate title, decide, and puts in the ground triangular flask, precision adds Diluted Alcohol 50ml, claims to decide weight, sonicated 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision pipettes subsequent filtrate 2ml, put in the 10ml measuring bottle, add moving phase, shake up to scale, filter with the 0.45um miillpore filter, make sample; Get adenine reference substance and adenosine reference substance, add Diluted Alcohol and make the solution that every 1ml contains 10ug respectively, in contrast product solution; Test according to high performance liquid chromatography, with octadecylsilane chemically bonded silica is filling agent, phosphate buffer solution with 0.5% tetrahydrofuran is a moving phase, the detection wavelength is 260nm, draw sample solution and each 20ul of reference substance solution, inject high performance liquid chromatograph, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, corresponding chromatographic peak is arranged;
Or b. gets capsule liquid 5g, put in the 10ml centrifuge tube, and in 12000 rev/mins hydro-extractor centrifugal 30 minutes, discard upper strata liquid, precipitation adds water 10ml, is heated to and boils, and filters, and gets subsequent filtrate as need testing solution; Other gets the alanine reference substance, adds water and makes the solution that every 1ml contains alanine 1mg, in contrast product solution; According to the thin-layered chromatography test, draw need testing solution 3ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with normal butyl alcohol-glacial acetic acid of 4: 1: 1-water is developping agent, launches, and takes out, dry, spray is with ninhydrin solution, and it is clear to be heated to the spot colour developing, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
Or c. gets the sweet mellow wine reference substance, adds Diluted Alcohol and makes the solution that every 1ml contains 9mg, in contrast product solution; Test according to thin-layered chromatography, drawing need testing solution and each 2ul of above-mentioned reference substance solution under the b item, put respectively on same silica gel g thin-layer plate, is developping agent with isopropyl alcohol-ethyl acetates of 9: 6: 2-water, launch, take out, dry, spray is with 2% liquor potassic permanganate, it is clear that hot blast blows to the spot colour developing, in the test sample chromatogram, with the relevant position of reference substance chromatogram on, show the spot of same color.
2, the effective constituent detection method of soft capsule as claimed in claim 1 is characterized in that this method comprises following content assaying method:
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; Phosphate buffer solution with 2% tetrahydrofuran is a moving phase; The detection wavelength is 260nm, number of theoretical plate is pressed the adenosine peak and is calculated, the preparation that should the be not less than 3000 reference substance solution 105 ℃ of drying under reduced pressure of learning from else's experience are an amount of to the adenosine reference substance of constant weight, the accurate title, decide, and adds Diluted Alcohol and make the solution that every 1ml contains 40ug, and precision pipettes 2ml, put in the 10ml measuring bottle, add moving phase to scale, shake up, promptly; The preparation of need testing solution is got capsule Huaihe River and is got 2.5g, and accurate the title decides, and puts in the ground triangular flask, precision adds Diluted Alcohol 50ml, claims to decide weight, sonicated 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, precision pipettes subsequent filtrate 2ml, put in the 10ml measuring bottle, add moving phase, shake up to scale, filter with the 0.45um miillpore filter, promptly; Accurate respectively reference substance solution and each 20ul of need testing solution of drawing of determination method injects high performance liquid chromatograph, measures, promptly.
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| CN100582771C true CN100582771C (en) | 2010-01-20 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102445514B (en) * | 2011-09-26 | 2014-08-20 | 江西济民可信集团有限公司 | Detection method of traditional Chinese medicine preparation jinshuibao capsule |
| CN108535372B (en) * | 2018-03-21 | 2020-10-09 | 江西国药有限责任公司 | Fermented cordyceps sinensis powder and preparation sterol HPLC fingerprint construction method and fingerprint thereof |
| CN108693276A (en) * | 2018-06-29 | 2018-10-23 | 江西济民可信药业有限公司 | A kind of fingerprint atlas detection method of Jinshuibao piece |
| CN109172618A (en) * | 2018-11-29 | 2019-01-11 | 江西济民可信金水宝制药有限公司 | A kind of pulsatile capsules |
| CN109172616A (en) * | 2018-11-29 | 2019-01-11 | 江西济民可信金水宝制药有限公司 | A kind of soft capsule and preparation method thereof |
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