CN109254098A - A kind of method of quality control of ' Qianjin ' capsule to treat ganopathy - Google Patents
A kind of method of quality control of ' Qianjin ' capsule to treat ganopathy Download PDFInfo
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Abstract
The invention discloses a kind of method of quality control of ' Qianjin ' capsule to treat ganopathy.Described method includes following steps: clear cream prepared by eight kinds of raw materials is mixed and detected, control genistin, the total amount of jateorrhizine, palmatine, jamaicin, Z- Ligustilide, Z-3- butylidene phthalide, andrographolide and Dehydro and drographolide in clear cream, it is spray-dried, then it pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy.Method of quality control of the present invention is on existing standards of pharmacopoeia, increase Six-element core component content, establish the new standard of quality control, the ' Qianjin ' capsule to treat ganopathy prepared using the control method, same effect is more stable between different batches, and ' Qianjin ' capsule to treat ganopathy provided by the present invention has better clinical therapeutic efficacy compared to the prior art.
Description
Technical field
The present invention relates to technical field of traditional Chinese medicines, more particularly, to a kind of method of quality control of ' Qianjin ' capsule to treat ganopathy.
Background technique
' Qianjin ' capsule to treat ganopathy is by philippine flemingia root, cherokee rose root, Herba Andrographitis, leatherleaf mahonia, single side needle, Radix Angelicae Sinensis, Caulis Spatholobi, Radix Codonopsis 8
Drug made of taste medicinal material.Effect is removing damp-heat, tonifying Qi and blood.For vaginal discharge diseases caused by dampness and heat stasis, abdominal pain symptoms include band
Lower amount is more, color Huang matter is thick, smelly dirty, underbelly pain, waist sacrum ache, spiritlessness and weakness；Chronic pelvic inflammatory disease, endometritis, chronic palace
Neck inflammation is shown in above-mentioned patient.
In existing Chinese Pharmacopoeia, the content of ' Qianjin ' capsule to treat ganopathy is identified, is only to define in wherein Herba Andrographitis
The total content of ester and Dehydro and drographolide, specifically in every capsule, containing Herba Andrographitis with andrographolide (C20H30O5) and
Dehydro and drographolide (C20H28O4) total amount meter, 1.6mg must not be less than.And in the compatibility ingredient of ' Qianjin ' capsule to treat ganopathy, it wears
Heart lotus is as just ministerial drug therein, it is clear that existing standard does not carry out other important components in ' Qianjin ' capsule to treat ganopathy
Regulation, so that the same effect between control ' Qianjin ' capsule to treat ganopathy different batches of product has difficulties.Match although having passed through
Side and preparation method obtain relatively consistent product, but need a kind of more effective means still to improve gynaecology's a thousand pieces of gold
The therapeutic effect of capsule.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the defect of the above-mentioned prior art and deficiencies, provide a kind of gynaecology's a thousand pieces of gold
The method of quality control of capsule.Using the ' Qianjin ' capsule to treat ganopathy of method of quality control of the present invention preparation relative to existing woman
Section's a thousand pieces of gold capsule shows more stable in terms of same effect, and relative to existing ' Qianjin ' capsule to treat ganopathy, has better
Clinical therapeutic efficacy.
Above-mentioned purpose of the invention is achieved by following scheme:
A kind of method of quality control of ' Qianjin ' capsule to treat ganopathy, the method for quality control include the following steps:
Using very heavy group, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as raw material；
S1. clear cream is made in the extraction of Radix Angelicae Sinensis alcohol percolation method first；
S2. clear cream is made in the extraction of Herba Andrographitis ethanol refluxing process；
S3. leatherleaf mahonia, single side needle boiling are extracted twice, the two filtrate is merged clear cream is made after filtering；
S4. primary rear filtering is extracted into very heavy group, cherokee rose root, Caulis Spatholobi, Radix Codonopsis boiling, by the filtered dregs of a decoction and step
The leatherleaf mahonia of the Radix Angelicae Sinensis dregs of a decoction, the Herba Andrographitis dregs of a decoction that step S2 is generated and step S3 generation that S1 is generated and single side medicine administered by injection slag are together
Simultaneously clear cream is made in boiling, filtering, merging filtrate；
S5. merge tetra- kinds of clear creams of above-mentioned S1, S2, S3, S4, mix, control Z- Ligustilide and Z-3- cyclobutenyl in clear cream
The content and andrographolide of at least one of phthalide and the total amount of Dehydro and drographolide reach standard content, carry out
Then spray drying pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy.According in 2015 editions Pharmacopoeias of the People's Republic of China
Regulation, the quality of every ' Qianjin ' capsule to treat ganopathy is 0.4mg.
In the ' Qianjin ' capsule to treat ganopathy, philippine flemingia root, leatherleaf mahonia are clearing heat and detoxicating, eliminating dampness stops band, are altogether monarch drug in a prescription；Herba Andrographitis, list
Face needle is clearing heat and detoxicating, cool blood detumescence, eliminating dampness stops band, is ministerial drug；Caulis Spatholobi, Chinese Angelica blood replonishing promoting blood circulation；Radix Codonopsis replenishes qi to invigorate the spleen, and promotes water
Wet transporting and stop-band；Cherokee rose root treating spontaneous emission and leukorrhagia is altogether adjutant.
Chinese medicine compound prescription is the organic whole having levels with structure, and effect is not the simple adduction of each simple,
But it is that multiple active constituents cooperate jointly between each other as a result, and being advised in existing pharmacopeia for the standard of ' Qianjin ' capsule to treat ganopathy
It is fixed only to define that andrographolide and two kinds of Dehydro and drographolide from ministerial drug (from Herba Andrographitis), and do not limit other
The type and content of effective component.And in the actual production process, due to only having detected Herba Andrographitis in quality testing and control
Lactone and Dehydro and drographolide, and the type and content of other effective components are not detected.And it is well known that Chinese medicinal material extract
The content of middle effective component is that the influence of region and extracting method is planted by medicinal material, even therefore according to identical
The extract of composition of raw materials preparation, wherein the content of certain specific effective component is different.Therefore, different batches produce
The content for other effective components not detected between ' Qianjin ' capsule to treat ganopathy be it is skimble-scamble, then leading to its drug effect, there are biggish differences
It is different.
In order to guarantee in the actual production process, the drug effect of the ' Qianjin ' capsule to treat ganopathy of preparation is consistent, and inventor is by multiple
Test discovery, other than andrographolide and Dehydro and drographolide, it is ensured that genistin, jateorrhizine, bar horse in product
Spit of fland, jamaicin, Z- Ligustilide and Z-3- butylidene phthalide this 6 kinds of effective components content in a certain range when, production
The effect of product is preferable, and the drug effect between different batches is with uniformity, and clinical therapeutic efficacy gets a promotion.Due in
There are various factors in medicine preparation process, the core component content in Chinese medicine is controlled, can overcome different batches it
Between, component content fluctuate the problem of.
Preferably, the content of Z- Ligustilide is no less than 0.01mg and/or Z-3- butylene in every milligram of clear cream in step S5
The content of base phthalide is no less than 0.00017mg and andrographolide and the total amount of Dehydro and drographolide is no less than 0.01mg.
Preferably, the content of Z- Ligustilide is no less than 0.015mg and/or Z-3- butylene in every milligram of clear cream in step S5
The content of base phthalide is no less than 0.00025mg and andrographolide and the total amount of Dehydro and drographolide is no less than
0.015mg。
Preferably, the content of Z- Ligustilide is 0.0165~0.022mg and/or Z-3- in every milligram of clear cream in step S5
The content of butylidene phthalide is many for the total amount of 0.00036~0.0006mg and andrographolide and Dehydro and drographolide
In 0.02mg.
A kind of method of quality control of ' Qianjin ' capsule to treat ganopathy, the method for quality control include the following steps:
Using very heavy group, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as raw material；
S1. clear cream is made in the extraction of Radix Angelicae Sinensis alcohol percolation method first；
S2. clear cream is made in the extraction of Herba Andrographitis ethanol refluxing process；
S3. leatherleaf mahonia, single side needle boiling are extracted twice, the two filtrate is merged clear cream is made after filtering；
S4. primary rear filtering is extracted into very heavy group, cherokee rose root, Caulis Spatholobi, Radix Codonopsis boiling, by the filtered dregs of a decoction and step
The leatherleaf mahonia of the Radix Angelicae Sinensis dregs of a decoction, the Herba Andrographitis dregs of a decoction that step S2 is generated and step S3 generation that S1 is generated and single side medicine administered by injection slag are together
Simultaneously clear cream is made in boiling, filtering, merging filtrate；
S5. merge tetra- kinds of clear creams of above-mentioned S1, S2, S3, S4, mix, control clear cream in Z- Ligustilide content, and/or
The content of the content of Z-3- butylidene phthalide, and/or the content, and/or palmatine of the content of genistin, and/or jateorrhizine,
And/or the content and andrographolide of jamaicin and the total amount of Dehydro and drographolide reach standard content, are sprayed
It is dry, it then pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy.According to the rule in 2015 editions Pharmacopoeias of the People's Republic of China
Fixed, the quality of every ' Qianjin ' capsule to treat ganopathy is 0.4mg.
Preferably, the content of genistin is no less than the content of 0.00015mg, jateorrhizine in every milligram of clear cream in step S5
No less than 0.0004mg, palmatine content be no less than 0.00038mg, the content of jamaicin is no less than 0.0004mg, Z- rhizoma ligustici
The content that the content of lactone is no less than 0.01mg, Z-3- butylidene phthalide is no less than 0.00017mg, andrographolide and dehydration and wears
The total amount of heart lotus lactone is no less than 0.01mg.
Preferably, the content of genistin is no less than the content of 0.0002mg, jateorrhizine in every milligram of clear cream in step S5
No less than 0.0006mg, palmatine content be no less than 0.0006mg, the content of jamaicin is no less than in 0.0006mg, Z- rhizoma ligustici
The content that the content of ester is no less than 0.015mg, Z-3- butylidene phthalide is no less than 0.00025mg, andrographolide and dehydration and wears
The total amount of heart lotus lactone is no less than 0.015mg.
Preferably, the content that genistin described in every milligram of clear cream is controlled in S5 is 0.0025~0.0035mg, medicine root
The content of alkali is 0.009~0.015mg, the content of palmatine is 0.007~0.01mg, the content of jamaicin be 0.0085~
The content of 0.01mg, Z- Ligustilide is 0.0165~0.022mg, the content of Z-3- butylidene phthalide be 0.00036~
The total amount of 0.0006mg, andrographolide and Dehydro and drographolide are no less than 0.02mg.
Preferably, by every ' Qianjin ' capsule to treat ganopathy of the method preparation (according to 2015 editions " People's Republic of China (PRC)
Pharmacopeia " in regulation, the quality of every ' Qianjin ' capsule to treat ganopathy is 0.4mg) in genistin be no less than 0.025mg, jateorrhizine
No less than 0.08mg, palmatine are no less than 0.06mg, jamaicin is no less than 0.08mg, Z- Ligustilide and is no less than 2.0mg, Z-3-
The total amount that butylidene phthalide is no less than 0.03mg, andrographolide and Dehydro and drographolide is no less than 1.6mg.
Preferably, by every ' Qianjin ' capsule to treat ganopathy of the method preparation (according to 2015 editions " People's Republic of China (PRC)
Pharmacopeia " in regulation, the quality of every ' Qianjin ' capsule to treat ganopathy is 0.4mg) in genistin be no less than 0.032mg, jateorrhizine
No less than 0.12mg, palmatine are no less than 0.075mg, jamaicin is no less than 0.12mg, Z- Ligustilide and is no less than 2.6mg, Z-
The total amount that 3- butylidene phthalide is no less than 0.04mg, andrographolide and Dehydro and drographolide is no less than 2.5mg.
Preferably, the total amount of andrographolide and Dehydro and drographolide is no less than in every ' Qianjin ' capsule to treat ganopathy
3.5mg。
Preferably, by the dyewood containing 0.04~0.06mg in every ' Qianjin ' capsule to treat ganopathy of the method preparation
Glycosides, the jateorrhizine of 0.165~0.20mg, the palmatine of 0.090~0.130mg, the jamaicin of 0.13~0.18mg, 3.0~
Z-3- butylidene phthalide, andrographolide and the Dehydro and drographolide of the Z- Ligustilide of 3.65mg, 0.065~0.105mg
Total amount be no less than 3.5mg.
Preferably, in S5, the control is the extraction process or raw material sources by adjusting S1, S2, S3, S4, so that
The mixed genistin of four kinds of clear creams, jateorrhizine, palmatine, jamaicin, Z- Ligustilide and the Z-3- cyclobutenyl of S1~S4
The content of phthalide reaches the range of needs.
Preferably, the method for the S1 is that Radix Angelicae Sinensis is ground into coarse powder, crosses 8 meshes, is soaked with the ethyl alcohol that mass concentration is 70%
Profit, is fitted into percolator, impregnates 48h, carries out diacolation with the speed of 0.2mL/min, collects the percolate of 10 times of amounts, be concentrated to get
Relative density is 1.1 (80 DEG C), as Radix Angelicae Sinensis clear cream.
Preferably, the method for the S2 are as follows: Herba Andrographitis crushing is sieved with 100 mesh sieve, is that 1:9 addition quality is dense according to solid-liquid ratio
The ethyl alcohol heating and refluxing extraction that degree is 90%, flow back 4h, extraction fluid, and then the dregs of a decoction are 1:8 reflux according still further to solid-liquid ratio
3.5h, extraction fluid merge extracting solution twice, and filtering is concentrated to get the Herba Andrographitis clear cream that relative density is 1.1 (80 DEG C).
Preferably, the method for the S3 is to extract leatherleaf mahonia, single side needle boiling twice, adds two taste Chinese medicine gross weights for the first time
The water for measuring 12 times of amounts decocts 4h, and decocting liquid is released, and the water of second plus 10 times amount decocts 3 hours, and decocting liquid is released, collecting decoction, filter
It crosses, filtrate is concentrated to get the clear cream that relative density is 1.1 (80 DEG C).
Preferably, the method for the S4 is that philippine flemingia root, cherokee rose root, Caulis Spatholobi, Radix Codonopsis are added boiling according to solid-liquid ratio 1:10
3.5h extracts primary rear filtering, and filtrate is concentrated to get the clear cream that relative density is 1.1 (80 DEG C), by the filtered dregs of a decoction and step
The dregs of a decoction that the Herba Andrographitis dregs of a decoction, the step S3 of the Radix Angelicae Sinensis dregs of a decoction, step S2 generation that rapid S2 is generated are generated merge, and add 4 times of volume decoctings
3h is boiled, is filtered, the clear cream that relative density is 1.1 (80 DEG C) is concentrated to get.
Preferably, detecting step described in S5 are as follows: take 1g clear cream that 75% methanol aqueous solution of 200mL is added to dissolve, then take 2mL
75% methanol aqueous solution of lysate, ultrasonic extraction (30 ± 5) min are supplied with 75% methanol aqueous solution and are subtracted after being down to room temperature
Quality is lost, 0.45 μm of miillpore filter is crossed, takes filtrate as solution to be measured；
Using Kromasil 100-5-C18 chromatographic column (250mm × 4.6mm, 5 μm), mobile phase using acetonitrile as A phase and
0.1% phosphate aqueous solution is as B phase, gradient elution, flow velocity 1.0mLmin-1, Detection wavelength 254nm, (30 ± 0.5)
DEG C, sample volume is 10 μ L.
Preferably, the genistin come from ' Qianjin ' capsule to treat ganopathy raw medicinal material philippine flemingia root, the jateorrhizine, palmatine and
Jamaicin comes from ' Qianjin ' capsule to treat ganopathy raw medicinal material leatherleaf mahonia, and the Z- Ligustilide and Z-3- butylidene phthalide come from gynaecology thousand
Gold size capsule raw medicinal material Radix Angelicae Sinensis, the andrographolide and Dehydro and drographolide come from ' Qianjin ' capsule to treat ganopathy raw medicinal material punching
Lotus.
Preferably, the dosage of Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis and single side needle is respectively the 9% of medicinal material total amount；Cherokee rose root, Caulis Spatholobi,
The dosage of leatherleaf mahonia and philippine flemingia root is respectively the 16% of medicinal material total amount.
The present invention also protects the ' Qianjin ' capsule to treat ganopathy prepared by above-mentioned method of quality control simultaneously and its treats woman in preparation
In application in section's disease.
Preferably, the gynecological disease is chronic pelvic inflammatory disease, chronic appendages inflammation or endometritis.
Compared with prior art, the invention has the following advantages:
The present invention joined detection process in the preparation process of product, by chemical component in ' Qianjin ' capsule to treat ganopathy
Analysis, establishes the new standard of control ' Qianjin ' capsule to treat ganopathy quality, which increases other cores on existing standards of pharmacopoeia
Heart component content, according to ' Qianjin ' capsule to treat ganopathy made of the range, same effect is more stable between different batches, and with
Core component type limits more, and drug effect consistency is more stable；And ' Qianjin ' capsule to treat ganopathy provided by the present invention, is compared
In the prior art, there is better clinical therapeutic efficacy.
Meanwhile the present invention is detected using HPLC method, not only testing result accuracy is high, and detection process is quick, simple
It is single, in the actual production process convenient for ' Qianjin ' capsule to treat ganopathy of the present invention, it can be detected simultaneously in original preparation process
With the content of monitoring plurality of active ingredients, be conducive to the execution of new standard.
Specific embodiment
The present invention is made combined with specific embodiments below and further being elaborated, the embodiment is served only for explaining this
Invention, is not intended to limit the scope of the present invention.Test method as used in the following examples is normal unless otherwise specified
Rule method；Used material, reagent etc., unless otherwise specified, for the reagent and material commercially obtained.
1 ' Qianjin ' capsule to treat ganopathy of embodiment
The formula of ' Qianjin ' capsule to treat ganopathy: Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis and single side needle dosage be respectively the 9% of medicinal material total amount；Gold
Cherry root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root dosage be respectively the 16% of medicinal material total amount.Medicinal material total amount is 500kg.By with lower section
Method prepares product:
(1) clear cream is made in the extraction of Radix Angelicae Sinensis alcohol percolation method first: Radix Angelicae Sinensis is ground into coarse powder, crosses 8 meshes, dense with quality
Degree infiltrates for 70% ethyl alcohol, is fitted into percolator, impregnates 48h, carries out diacolation with the speed of 0.2mL/min, collects 10 times of amounts
Percolate, being concentrated to get relative density is 1.1 (80 DEG C), as Radix Angelicae Sinensis clear cream；
(2) clear cream is made in the extraction of Herba Andrographitis ethanol refluxing process: Herba Andrographitis crushing is sieved with 100 mesh sieve, according to solid-liquid ratio
The ethyl alcohol heating and refluxing extraction that mass concentration is 90% is added for 1:9, flow back 4h, and extraction fluid, then the dregs of a decoction are according still further to material
Liquor ratio is 1:8 reflux 3.5h, and extraction fluid, combined extract, filtering, being concentrated to get relative density is 1.1 (80 DEG C), as
Herba Andrographitis clear cream；
(3) leatherleaf mahonia, single side needle boiling are extracted twice, for the first time plus the water of 12 times of two taste Chinese medicine total weights amounts decocts
4h, decocting liquid are released；The water of second plus 10 times of two taste Chinese medicine total weights amount decocts 3 hours, and decocting liquid is released, collecting decoction, filter
It crosses, relative density is 1.1 when filtrate is concentrated into 80 DEG C, obtains the clear cream of two taste medicines；
(4) it is that 1:10 adds boiling 3.5h according to solid-liquid ratio by very heavy group, cherokee rose root, Caulis Spatholobi, Radix Codonopsis, extracts primary rear mistake
Filter, relative density is the clear cream of 1.1 (80 DEG C) when filtrate is concentrated into 80 DEG C；Then the filtered dregs of a decoction and step (1) are generated
The Radix Angelicae Sinensis dregs of a decoction, step (2) generate the Herba Andrographitis dregs of a decoction and step (3) generate leatherleaf mahonia, single side medicine administered by injection slag merge after plus 4 times
Volume of water decocts 3h, and filtering, relative density is the clear cream of 1.1 (80 DEG C) when filtrate is concentrated into 80 DEG C；
(5) merge above-mentioned (1), (2), (3), (4) four kinds of clear creams, mix, and carry out HPLC detection, control every milligram of clear cream
Described in Z- Ligustilide content be no less than 0.01mg, and/or Z-3- butylidene phthalide content be no less than 0.00017mg,
And/or the content of genistin is no less than 0.00015mg, and/or the content of jateorrhizine is no less than 0.0004mg, and/or bar horse
The content that the content in spit of fland is no less than 0.0038mg, and/or jamaicin is no less than 0.0004mg and andrographolide and wears with dehydration
The total amount of heart lotus lactone is no less than 0.01mg, is spray-dried, and then pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy,
The regulation of 2015 editions Pharmacopoeias of the People's Republic of China, the content of every ' Qianjin ' capsule to treat ganopathy are 0.4g.
In the testing result of the mixing clear cream of step (5), 6 kinds of effective components (Z- Ligustilides, Z-3- cyclobutenyl benzene
Phthalein, genistin, jateorrhizine, palmatine, jamaicin) in the content of any ingredient when being unsatisfactory for above-mentioned condition, retain part
Sample is spare.
In the testing result of the mixing clear cream of step (5), 6 kinds of effective components (Z- Ligustilides, Z-3- cyclobutenyl benzene
Phthalein, genistin, jateorrhizine, palmatine, jamaicin) content when being all unsatisfactory for above-mentioned condition, be contrast sample, it is spare.
The clear cream Producing reason for analyzing active constituent content fluctuation, may have due to the raw medicinal material between different batches
Caused by effective component content is different.
' Qianjin ' capsule to treat ganopathy is prepared referring to the above method, the production of multiple batches is randomly selected from long-term, a large amount of product
Product, and HPLC detection is carried out to the ' Qianjin ' capsule to treat ganopathy product of each batch:
The preparation of test solution: randomly selecting ' Qianjin ' capsule to treat ganopathy, takes out content 1.0g, is placed in the three of tool grinding port plug
In the bottle of angle, 75% methanol aqueous solution of 20mL, weighed, ultrasonic extraction 30min, after being down to room temperature, with 75% first is added in precision
Alcohol solution supplies less loss quality, crosses 0.45 μm of miillpore filter, takes filtrate as test solution.
Using Kromasil 100-5-C18 chromatographic column (250mm × 4.6mm, 5 μm), mobile phase be acetonitrile (A phase) and
0.1% phosphate aqueous solution (B phase), gradient elution, flow velocity 1.0mLmin-1, Detection wavelength 254nm, column temperature is 30 DEG C, into
Sample amount is 10 μ L.
Embodiment 2
A kind of ' Qianjin ' capsule to treat ganopathy, step (1) to (4) is with embodiment 1 in preparation process, the difference is that step
(5), the content for controlling Z- Ligustilide described in every milligram of clear cream is no less than containing for 0.015mg, and/or Z-3- butylidene phthalide
The amount no less than content of 0.00025mg, and/or genistin is no less than 0.002mg, and/or the content of jateorrhizine is no less than
The content of 0.006mg, and/or palmatine is no less than 0.006mg, and/or the content of jamaicin is no less than 0.006mg and wears
The total amount of heart lotus lactone and Dehydro and drographolide is no less than 0.015mg, is spray-dried, and then pelletizes, is canned, obtaining institute
' Qianjin ' capsule to treat ganopathy is stated, the content of the regulation of 2015 editions Pharmacopoeias of the People's Republic of China, every ' Qianjin ' capsule to treat ganopathy is
0.4g。
' Qianjin ' capsule to treat ganopathy is prepared referring to the above method, the production of multiple batches is randomly selected from long-term, a large amount of product
Product, and the ' Qianjin ' capsule to treat ganopathy product of each batch is detected referring to the HPLC detection method in embodiment 1.
It is selected at random from multiple batch samples that embodiment 1 detects and selects 6 batches in 6 batches and embodiment 2 at random
Secondary progress HPLC detection, testing result are shown in Table 1.
Eight kinds of component contents (μ g/) in ' Qianjin ' capsule to treat ganopathy prepared by 1 embodiment 1 of table, embodiment 2
1 ' Qianjin ' capsule to treat ganopathy of comparative example
Choose Z- Ligustilide, Z-3- butylidene phthalide, genistin, jateorrhizine, palmatine and jamaicin in embodiment 1
Content do not meet embodiment 1 requirement clear cream, be directly spray-dried, then granulation, it is canned, obtain the gynaecology thousand
Gold size capsule, the regulation of 2015 editions Pharmacopoeias of the People's Republic of China, the content of every ' Qianjin ' capsule to treat ganopathy are 0.4g.And to each
The ' Qianjin ' capsule to treat ganopathy product of batch carries out HPLC detection using identical method.
With embodiment 1, testing result is as shown in table 2 for testing conditions and method.
Eight kinds of component contents (μ g/) in the ' Qianjin ' capsule to treat ganopathy of 2 comparative example 1 of table preparation
| Batch 1 | Batch 2 | Batch 3 | Batch 4 | |
| Genistin/mg | 24.35±0.46 | 21.33±0.25 | 24.21±0.23 | 18.08±1.11 |
| Jateorrhizine/mg | 71.56±0.16 | 76.35±1.68 | 67.84±1.22 | 58.26±2.63 |
| Palmatine/mg | 55.33±1.23 | 51.32±0.26 | 48.76±0.25 | 59.03±1.07 |
| Jamaicin/mg | 75.10±0.22 | 54.10±0.42 | 73.26±0.32 | 69.16±0.56 |
| Andrographolide/mg | 1380.26±10.38 | 1131.26±7.18 | 1065.56±5.62 | 1166.61±14.02 |
| Dehydro and drographolide/mg | 568.72±8.85 | 651.04±0.54 | 718.24±0.32 | 562.58±10.22 |
| Z- Ligustilide/mg | 1684.02±2.35 | 1700.34±2.05 | 1573.36±5.16 | 1710.25±1.68 |
| Z-3- butylidene phthalide/mg | 23.31±0.24 | 18.35±1.20 | 28.15±1.16 | 25.21±1.67 |
As can be known from Table 2, in the ' Qianjin ' capsule to treat ganopathy according to the preparation of existing method, in addition to andrographolide and dehydration are worn
The content of heart lotus lactone meets outside the regulation in pharmacopeia, the content of other effective components between batch there are biggish difference,
It is easy to cause the unstable of drug effect.
The test of 3 pharmacy in vitro of embodiment
The drug or material of use: croton oil, by Nanjing, institute of internal medicine is provided；Carrageenan, Japan and the pure medicine of light
Industrial Co., Ltd's production；Nutrient broth medium, Huankai Microbes Tech Co., Ltd., Guangdong's product；Mould medium, by
Nat'l Pharmaceutical & Biological Products Control Institute provides.
A thousand pieces of gold capsule of embodiment 1 (batch 1 and batch 6) and comparative example 1 (batch 1) preparation is respectively adopted as sample.
Used cleaning grade Kunming mouse, SD rat are provided by Hunan Drug Testing Institute；Escherichia coli ATCC25922, gold
Staphylococcus aureus ATCC25923, hemolytic chain bacterium ATCC32172, is provided by Hunan Hygienic & Epidemic Prevention Station, and white is read
Pearl bacterium is provided by being clinically separated by Annex III institute of Hunan Medical University clinical laboratory Bacteriology Room.
1) to the extracorporeal bacteria inhibitor test of standard bacteria
As a result as shown in table 3 to table 5.
The 1 ' Qianjin ' capsule to treat ganopathy bacteriostatic test result (liquid tube method) of batch of 3 embodiment 1 of table
The 6 ' Qianjin ' capsule to treat ganopathy bacteriostatic test result (liquid tube method) of batch of 4 embodiment 1 of table
5 comparative example of table, 1 batch, 1 ' Qianjin ' capsule to treat ganopathy bacteriostatic test result (liquid tube method)
==indicates that two groups repeat test without bacterial growth ,+, ++, +++ respectively indicate the growth degree of cell
Table 3 is to table 5 the results showed that the ' Qianjin ' capsule to treat ganopathy of embodiment 1 and comparative example 1 is to Escherichia coli, golden yellow
The minimal inhibitory concentration of staphylococcus, beta hemolytic streptococcus and Candida albicans is respectively 12.5,6.25,12.5,12.5,
The two Mlc is consistent.
2) to the antibacterial experiment in vitro for being clinically separated pathogenic bacteria
Escherichia coli, staphylococcus aureus, beta hemolytic streptococcus, Candida albicans are obtained by clinical patient separation
, and identify through bacteriology, it is provided by the attached three institute's clinical laboratory Bacteriology Room of institute of Hunan Medical University.
As a result as shown in table 6 to table 8.
1 ' Qianjin ' capsule to treat ganopathy of batch of 6 embodiment 1 of table is to the bacteriostatic experiment result (liquid tube method) being clinically separated
| Bacterial strain | Strain number (strain) | Bacterial concentration (GFu/mL) | Minimal inhibitory concentration (%) |
| Escherichia coli | 32 | 105~106 | 50.0~25.0 |
| Staphylococcus aureus | 23 | 105~106 | 12.5~3.13 |
| Beta hemolytic streptococcus | 20 | 105~106 | 50.0~25.0 |
| Candida albicans | 27 | 105~106 | 12.5~3.13 |
6 ' Qianjin ' capsule to treat ganopathy of batch of 7 embodiment 1 of table is to the bacteriostatic experiment result (liquid tube method) being clinically separated
| Bacterial strain | Strain number (strain) | Bacterial concentration (GFu/mL) | Minimal inhibitory concentration (%) |
| Escherichia coli | 32 | 105~106 | 50.0~25.0 |
| Staphylococcus aureus | 23 | 105~106 | 12.5~3.13 |
| Beta hemolytic streptococcus | 20 | 105~106 | 50.0~25.0 |
| Candida albicans | 27 | 105~106 | 12.5~3.13 |
8 comparative example of table, 1 batch, 1 ' Qianjin ' capsule to treat ganopathy is to the bacteriostatic experiment result (liquid tube method) being clinically separated
| Bacterial strain | Strain number (strain) | Bacterial concentration (GFu/mL) | Minimal inhibitory concentration (%) |
| Escherichia coli | 32 | 105~106 | 50.0~25.0 |
| Staphylococcus aureus | 23 | 105~106 | 12.5~3.13 |
| Beta hemolytic streptococcus | 20 | 105~106 | 50.0~25.0 |
| Candida albicans | 27 | 105~106 | 12.5~3.13 |
Table 6 is to table 8 the results showed that embodiment 1 and the ' Qianjin ' capsule to treat ganopathy of the preparation of comparative example 1 are to four be clinically separated
Kind bacterium has identical inhibiting effect, and effect is consistent.
3) internal bacteriostatic experiment
Protective effect to mouse infection Escherichia coli: taking Kunming mouse 150, male and female dual-purpose, 20~22g of weight,
It is divided into 15 groups (n=10), five groups of ' Qianjin ' capsule to treat ganopathy for 1 batch 1 of embodiment, five groups of woman for 1 batch 6 of embodiment
Section's a thousand pieces of gold capsule, five groups of ' Qianjin ' capsule to treat ganopathy for 1 batch 1 of comparative example, dosage is respectively 17.3,24.7,35.3,50.4
With 72.0g crude drug/kg.
Stomach-filling is 0.5mL/20g to volume, and each group upon administration one hour, every mouse injected 0.5mL large intestine bar
Bacterium (106FGu/mL) hold soup culture solution, 12 hours and 24 hours after mouse infection bacterium, then be administered secondary, then observe seven
It, records animal dead number.Animal dead peak is after 24 hours between 48 hours.
Protective effect of 9 ' Qianjin ' capsule to treat ganopathy of table to coli-infection mouse
Table 9 the results showed that the ' Qianjin ' capsule to treat ganopathy for preparing of embodiment 1 and comparative example 1 to coli-infection mouse
High dose group all has certain protective effect.
4) anti-inflammatory effect (influence to croton oil induced mice swelling)
Stand-by medicine ordinance: taking the content of stand-by ' Qianjin ' capsule to treat ganopathy, is made into the outstanding of various concentration with distilled water respectively
Supernatant liquid, for mouse, daily progress gastric infusion is primary, and stomach-filling medical fluid is ready-to-use.
Mouse 100, male, 24~26g of weight is divided into 10 groups (n=10), and the medicine of various concentration is given in stomach-filling respectively
Liquid, the isometric distilled water of control group stomach-filling, once a day, totally 7 days, last dose 1 hour, every mouse auris dextra applied 2% croton oil
(2% croton oil, 20% dehydrated alcohol, 5% distilled water and 73% ether) 0.1mL, all left ears of mouse are without any processing；Altogether
Cervical dislocation puts to death mouse after administration 7 days, last dose 4 hours, cuts ears, and punching weighing calculates every group of mouse swelling.
Influence (X ± SD, n=10) of 10 ' Qianjin ' capsule to treat ganopathy of table to croton oil induced mice ear swelling
Compared with the control group, * P > 0.05, * * P < 0.05, * * * P < 0.01
Table 10 the result shows that: ' Qianjin ' capsule to treat ganopathy prepared by embodiment 1 and comparative example 1 compared with the control group, can be obvious
Inhibit croton oil induced mice ear swelling；But the inhibitory effect of 2 batches is substantially better than the gynaecology thousand of comparative example 1 in embodiment 1
Gold size capsule.
5) to the influence of rat paw edema caused by Irish moss
SD rat 70, male is divided into seven groups (n=10), and the medical fluid of various concentration is given in stomach-filling respectively, and control group fills
The isometric distilled water of stomach, once a day, totally seven days, last dose 1 hour, in Rat Right vola pedis bottom injection Irish moss
0.1mL/ only causes inflammation.It is administered once again within 2 hours after causing inflammation, in addition to normal vola pedis size before measurement cause inflammation, every 1 hour after cause is scorching
Vola pedis size is surveyed, totally 6 times, calculates swelling.
The influence (X ± cm, n=10) that 11 ' Qianjin ' capsule to treat ganopathy of table swells to vola pedis caused by Rat Carrageenan
Compared with the control group, * P > 0.05, * * P < 0.05, * * * P < 0.01
Table 11 the result shows that: ' Qianjin ' capsule to treat ganopathy prepared by embodiment 1 and comparative example 1 compared with the control group, can be obvious
Inhibit rat paw edema caused by Irish moss；But the ' Qianjin ' capsule to treat ganopathy of 2 batches is for the foot of rat caused by Irish moss in embodiment 1
The inhibiting effect of swelling is better than the ' Qianjin ' capsule to treat ganopathy of comparative example 1, in 3~4h period especially after medication.
6) influence of Dichlorodiphenyl Acetate induced pain mouse
Mouse 100 are taken, half male and half female, 20~22g of weight is randomly divided into 10 groups (n=10), and difference is given in stomach-filling respectively
The medical fluid of concentration, the isometric distilled water of control group stomach-filling, one hour after administration, every mouse injected 0.6% acetic acid
0.2mL/ is only.Start recording after injection 5min, records mouse writhing number in 10 minutes.
The influence (X ± SD, n=10) of 12 ' Qianjin ' capsule to treat ganopathy Dichlorodiphenyl Acetate induced pain mouse of table
Compared with the control group, * * P < 0.05, * * * P < 0.01
Table 12 the result shows that: ' Qianjin ' capsule to treat ganopathy prepared by embodiment 1 and comparative example 1 compared with the control group, can be significant
Reduce acetic acid induced pain mouse writhing number；But the ' Qianjin ' capsule to treat ganopathy of 2 batches is bright for the effect of acetic acid induced pain in embodiment 1
The aobvious ' Qianjin ' capsule to treat ganopathy better than comparative example 1.
7) to the influence of the hot plate method induced pain mouse threshold of pain
The mouse threshold of pain is measured as follows: under room temperature at 20 ± 1 DEG C, mouse being placed in 55 ± 0.5 DEG C
On hot plate, to contact hot plate to licking the metapedes time experienced as pain threshold.
Then female mice of the threshold of pain less than 30 seconds 100, weight 20-22g is taken, 10 groups (n=10) are divided into, by acetic acid
The disposable gastric infusion of dosage in induced pain mouse, by said determination method, at 55 ± 0.5 DEG C before measurement administration and after administration
30,60 and 90 minutes pain thresholds, the results are shown in Table 13.
Influence (X ± SD, n=10) of 13 ' Qianjin ' capsule to treat ganopathy of table to the hot plate method induced pain mouse threshold of pain
Control group compares, * * P < 0.05, * * * P < 0.01
Table 13 the result shows that, ' Qianjin ' capsule to treat ganopathy prepared by embodiment 1 and comparative example 1 compared with the control group, can be obvious
Improve the threshold of pain of hot plate excitement induced pain mouse；But the ' Qianjin ' capsule to treat ganopathy of 2 batches is to hot plate excitement induced pain mouse in embodiment 1
The raising percentage of the threshold of pain be apparently higher than the ' Qianjin ' capsule to treat ganopathy of comparative example 1.
8) to the influence of blood loss type deficiency of blood mouse
Mouse 110, male and female dual-purpose, 20~22g of weight is divided into 11 groups (n=10), take first blood survey mouse RBC and
The normal value of HB, then in addition to Normal group, other groups of every mouse are from orbital venous plexus bloodletting 0.5mL, after 24 hours again
Blood is taken to survey the value of mouse RBC and HB, then by stomach-filling to the medicine of various dose, once a day, totally seven days, 24 is small after the last administration
When, mouse orbit veniplex takes blood to survey RBC and HB value, the results are shown in Table 14.
Influence (X ± SD, n=10) of 14 ' Qianjin ' capsule to treat ganopathy of table to blood loss type deficiency of blood mouse
With model group compared with, * P < 0.05, * * P < 0.01
Table 14 the result shows that, ' Qianjin ' capsule to treat ganopathy prepared by embodiment 1 and comparative example 1 compared with the control group, to blood loss
Property deficiency of blood mouse have apparent blood tonification effect；But the ' Qianjin ' capsule to treat ganopathy of 2 batches is to Lost blood anemia mouse in embodiment 1
Effect of enriching blood be apparently higher than the ' Qianjin ' capsule to treat ganopathy of comparative example 1.
Above-mentioned experimental result is taken a broad view of as it can be seen that the ' Qianjin ' capsule to treat ganopathy of embodiment 1 and comparative example 1 is to Escherichia coli, yellow Portugal
Grape bacterium, beta hemolytic streptococcus and the external minimal inhibitory concentration of Candida albicans, and it is thin to above-mentioned four kinds be clinically separated
Bacterium minimal inhibitory concentration is identical.
But in In-vivo test in mice, 2 batches in embodiment 1, comparative example 1 a thousand pieces of gold capsule can obviously inhibit croton oil
Rat paw edema caused by induced mice ear swelling and Irish moss；Acetic acid induced mice writhing number is reduced, hot plate method induced pain is improved
The threshold of pain of mouse；There can also be apparent blood tonification effect to Lost blood anemia mouse；But the woman that in embodiment 1 prepared by 2 batches
Above-mentioned effect of section's a thousand pieces of gold capsule relative to comparative example 1 ' Qianjin ' capsule to treat ganopathy have a degree of promotion, effect better than pair
The ' Qianjin ' capsule to treat ganopathy of ratio 1.
4 result in clinical application of embodiment:
In order to which the ' Qianjin ' capsule to treat ganopathy more of the invention for controlling plurality of active ingredients content and original method prepare gynaecology
The drug effect of a thousand pieces of gold capsule (i.e. comparative example 1) whether there is difference, carry out clinical test.Each testing site is centralized and unified according to related
The requirement of new drug research has drafted clinical research principle, has established diagnostic criteria, is included in standard, dumping standard, and taken this as the standard
Then, observation case is collected.The method of administration for abiding by specification appended by drug in use simultaneously, starts to take medicine when medical, and 7 days are one
The course for the treatment of, two courses for the treatment of of continuous use, and clinical symptoms and Signs variation are collected by the clinical observation table drafted.
Table 15 is that the second affiliated hospital of Hunan College of Traditional Chinese Medicine, the academy of traditional Chinese medicine of Hunan Province, Hunan Medical University first are attached
The clinical change after undergoing chronic pelvic inflammation takes two courses for the treatment of of ' Qianjin ' capsule to treat ganopathy is suffered to 240 using the drug by hospital etc.,
It is divided into 3 groups, every group of 80 patients.Concrete outcome is shown in Table 15.
The treatment of 15 undergoing chronic pelvic inflammation of table improves and proportion table
16~table of table 18 lists 240 and suffers from the effect statistics that adnexitis patient takes ' Qianjin ' capsule to treat ganopathy, and wherein table 16 is
240 adnexitis patient's gynecologial examination situations, 17 curative effect of table statistics, table 18 are the changes of symptom before and after taking ' Qianjin ' capsule to treat ganopathy
Situation.
16 adnexitis patient's gynecologial examination situation of table
| Position | Number of cases | Obvious tenderness | General tenderness | Light tenderness |
| Side adnexitis | 99 | 30 | 53 | 16 |
| Bilateral adnexitis | 141 | 63 | 60 | 18 |
| It is total | 240 | 93 | 113 | 34 |
17 adnexitis patient of table takes ' Qianjin ' capsule to treat ganopathy curative effect
18 adnexitis patient of table takes the change of symptom before and after ' Qianjin ' capsule to treat ganopathy
It is found that ' Qianjin ' capsule to treat ganopathy of the present invention is in terms for the treatment of chronic pelvic inflammatory disease and adnexitis from table 15~18
Effect is superior to the ' Qianjin ' capsule to treat ganopathy of comparative example, and wherein the effect of embodiment batch 6 is better than batch 1, the effect of embodiment batch 1
Fruit is due to being slightly better than 1 batch 1 of comparative example.Reflection is in addition to control Z- Ligustilide, Z-3- butylidene phthalide, andrographolide and takes off
Outside the content of water andrographolide, while genistin, jateorrhizine, palmatine, jamaicin are also controlled in critical field, treatment
Effect can be promoted further.
5 endometritis result in clinical application of embodiment
According to the good result that shows for the treatment of chronic pelvic inflammatory disease, we also directed to treatment endometritis curative effect into
Row comparison.608 cases of uterine inflammation patients are specifically chosen as research object, the age between 30~40 years old, therapeutic scheme
It is to give Antibiotic combination progestational hormone to be treated.0.5g metronidazole is added in 0.9% sodium chloride solution 250mL, vein
It instils, 1 time for every eight hours, takes within 3 days after menstruation medroxyprogesterone acetate, 5mg/ times, 2 times a day, take 14, and in this, as
Blank control group.Embodiment 1 (3 batches) and embodiment 2 (3 batches) are given on the basis of blank control group by observation group
' Qianjin ' capsule to treat ganopathy, control group give gynaecology's a thousand pieces of gold glue of comparative example 1 (3 batches) preparation on the basis of blank control group
Capsule.See Table 1 for details 9~21 for treatment results.
Evaluation criterion:
Effective: clinical symptoms disappear, and menstruation recovery is normal, and ultrasonic examination inflammation disappears；
Effective: clinical symptoms improve, and ultrasonic examination inflammation improves, endometrial thickness；
It is invalid: not have above-mentioned improvement.
19 Clinical efficacy comparison of table
20 menstruation recovery situation of table compares
21 ultrasound diagnosis of table recovery is compared
It can be seen that from the data of table 19~21 compared to the gynaecology's a thousand pieces of gold glue for only controlling Herba Andrographitis effective component originally
Capsule, the present invention control gynaecology's a thousand pieces of gold glue of genistin, and/or jateorrhizine, and/or palmatine, and/or content of berberine simultaneously
Capsule improves the effect of ' Qianjin ' capsule to treat ganopathy treatment endometritis, is embodied in efficient and obvious effective rate and gets a promotion, says
It is bright when controlling genistin, and/or jateorrhizine, and/or palmatine, and/or content of berberine, ' Qianjin ' capsule to treat ganopathy can with it is anti-
Raw element and progestational hormone have better mutual cooperation to act on.
It is tested from the consistency of above-described embodiment and comparative example as can be seen that in process of production, increasing to mixing clear cream
The detection of sample constituents, and control in reasonable range, 8 kinds of effective components in the ' Qianjin ' capsule to treat ganopathy obtained can be made
Content control is in reasonable a certain relatively narrow range, and consistency is more preferable between product batches obtained in this way, and clinical treatment
Effect gets a promotion.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of shield range can also be made on the basis of above description and thinking for those of ordinary skill in the art
Other various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (10)
1. a kind of method of quality control of ' Qianjin ' capsule to treat ganopathy, which is characterized in that the method for quality control includes the following steps:
Using very heavy group, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as raw material；
S1. clear cream is made in the extraction of Radix Angelicae Sinensis alcohol percolation method first；
S2. clear cream is made in the extraction of Herba Andrographitis ethanol refluxing process；
S3. leatherleaf mahonia, single side needle boiling are extracted twice, the two filtrate is merged clear cream is made after filtering；
S4. primary rear filtering is extracted into very heavy group, cherokee rose root, Caulis Spatholobi, Radix Codonopsis boiling, by the filtered dregs of a decoction and step S1
Leatherleaf mahonia that the Herba Andrographitis dregs of a decoction and step S3 that the Radix Angelicae Sinensis dregs of a decoction of generation, step S2 are generated generate and single side medicine administered by injection slag water together
It boils, filters, simultaneously clear cream is made in merging filtrate；
S5. merge tetra- kinds of clear creams of above-mentioned S1, S2, S3, S4, mix, control Z- Ligustilide and Z-3- butylidene phthalide in clear cream
At least one of content and the total amount of andrographolide and Dehydro and drographolide reach standard content, be sprayed
It is dry, it then pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy.
2. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 1, which is characterized in that in step S5 every milligram it is clear
The content that the content of Z- Ligustilide is no less than 0.01mg and/or Z-3- butylidene phthalide in cream be no less than 0.00017mg and
The total amount of andrographolide and Dehydro and drographolide is no less than 0.01mg；
Preferably, the content of Z- Ligustilide is no less than 0.015mg and/or Z-3- cyclobutenyl benzene in every milligram of clear cream in step S5
The content of phthalein is no less than 0.00025mg and andrographolide and the total amount of Dehydro and drographolide is no less than 0.015mg.
3. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 2, which is characterized in that in step S5 every milligram it is clear
In cream the content of Z- Ligustilide be 0.0165~0.022mg and/or the content of Z-3- butylidene phthalide be 0.00036~
The total amount of 0.0006mg and andrographolide and Dehydro and drographolide is no less than 0.02mg.
4. a kind of method of quality control of ' Qianjin ' capsule to treat ganopathy, which is characterized in that the method for quality control includes the following steps:
Using very heavy group, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as raw material；
S1. clear cream is made in the extraction of Radix Angelicae Sinensis alcohol percolation method first；
S2. clear cream is made in the extraction of Herba Andrographitis ethanol refluxing process；
S3. leatherleaf mahonia, single side needle boiling are extracted twice, the two filtrate is merged clear cream is made after filtering；
S4. primary rear filtering is extracted into very heavy group, cherokee rose root, Caulis Spatholobi, Radix Codonopsis boiling, by the filtered dregs of a decoction and step S1
Leatherleaf mahonia that the Herba Andrographitis dregs of a decoction and step S3 that the Radix Angelicae Sinensis dregs of a decoction of generation, step S2 are generated generate and single side medicine administered by injection slag water together
It boils, filters, simultaneously clear cream is made in merging filtrate；
S5. merge tetra- kinds of clear creams of above-mentioned S1, S2, S3, S4, mix, control the content, and/or Z-3- of Z- Ligustilide in clear cream
The content of the content of butylidene phthalide, and/or the content, and/or palmatine of the content of genistin, and/or jateorrhizine and/
Or the content and andrographolide of jamaicin and the total amount of Dehydro and drographolide reach standard content, are done by spraying
It is dry, it then pelletizes, is canned, obtaining the ' Qianjin ' capsule to treat ganopathy.
5. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 4, which is characterized in that in step S5 every milligram it is clear
The content of genistin is no less than 0.00015mg in cream, the content of jateorrhizine is no less than 0.0004mg, the content of palmatine is many
0.01mg, Z-3- butylene are no less than in the content that the content of 0.00038mg, jamaicin are no less than 0.0004mg, Z- Ligustilide
The total amount that the content of base phthalide is no less than 0.00017mg, andrographolide and Dehydro and drographolide is no less than 0.01mg；
Preferably, to be no less than 0.0002mg, the content of jateorrhizine many for the content of genistin in every milligram of clear cream in step S5
In the content of 0.0006mg, palmatine are no less than 0.0006mg, the content of jamaicin is no less than 0.0006mg, Z- Ligustilide
The content that content is no less than 0.015mg, Z-3- butylidene phthalide is no less than 0.00025mg, andrographolide and dehydration Herba Andrographitis
The total amount of lactone is no less than 0.015mg.
6. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 5, which is characterized in that control every milligram in S5 clearly
The content of genistin described in cream is 0.0025~0.0035mg, the content of jateorrhizine is 0.009~0.015mg, palmatine
Content be 0.007~0.01mg, the content of jamaicin is 0.0085~0.01mg, the content of Z- Ligustilide be 0.0165~
The content of 0.022mg, Z-3- butylidene phthalide is 0.00036~0.0006mg, andrographolide and Dehydro and drographolide
Total amount is no less than 0.02mg.
7. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 5, which is characterized in that by the method preparation
Every ' Qianjin ' capsule to treat ganopathy, the genistin contained is no less than 0.025mg, jateorrhizine is no less than 0.08mg, palmatine not
0.08mg, Z- Ligustilide are no less than less than 0.06mg, jamaicin are no less than 2.0mg, Z-3- butylidene phthalide be no less than
The total amount of 0.03mg, andrographolide and Dehydro and drographolide are no less than 1.6mg.
8. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 5, which is characterized in that by the method preparation
Every ' Qianjin ' capsule to treat ganopathy, the genistin contained is no less than 0.025mg, jateorrhizine is no less than 0.08mg, palmatine not
0.08mg, Z- Ligustilide are no less than less than 0.060mg, jamaicin are no less than 2.0mg, Z-3- butylidene phthalide be no less than
The total amount of 0.03mg, andrographolide and Dehydro and drographolide are no less than 1.9mg；
Preferably, by the method prepare every ' Qianjin ' capsule to treat ganopathy, the genistin contained be no less than 0.032mg,
Jateorrhizine is no less than 0.12mg, palmatine is no less than 0.075mg, jamaicin is no less than 0.12mg, Z- Ligustilide and is no less than
The total amount that 2.6mg, Z-3- butylidene phthalide are no less than 0.04mg, andrographolide and Dehydro and drographolide is no less than 2.5mg.
9. the method for quality control of ' Qianjin ' capsule to treat ganopathy according to claim 6, which is characterized in that by the method preparation
Every ' Qianjin ' capsule to treat ganopathy, the jateorrhizine of genistin, 0.165~0.20mg containing 0.04~0.06mg, 0.090~
The palmatine of 0.130mg, the jamaicin of 0.13~0.18mg, the Z- Ligustilide of 3.0~3.65mg, 0.065~0.105mg
The total amount of Z-3- butylidene phthalide, andrographolide and Dehydro and drographolide is no less than 3.5 mg.
10. according to claim 1 to the method for quality control of 9 any ' Qianjin ' capsule to treat ganopathy, which is characterized in that in step S5
The detection method used is HPLC detection；
Preferably, detecting step described in step S5 are as follows: take 1g clear cream that 75% methanol aqueous solution of 200mL is added to dissolve, then take 2mL molten
75% methanol aqueous solution of liquid is solved, ultrasonic extraction (30 ± 5) min supplies less loss with 75% methanol aqueous solution after being down to room temperature
Quality crosses 0.45 μm of miillpore filter, takes filtrate as solution to be measured；
Preferably, HPLC testing conditions in step S5 are as follows: use Kromasil 100-5-C18 chromatographic column (250 mm × 4.6
Mm, 5 μm), mobile phase is using acetonitrile as A phase and 0.1% phosphate aqueous solution as B phase, and gradient elution, flow velocity is 1.0 mL min-1, Detection wavelength is 254 nm, and column temperature is (30 ± 0.5) DEG C, and sample volume is 10 μ L；
Preferably, in S5, the control is the extraction process or raw material sources by adjusting S1, S2, S3, S4, so that S1~
The mixed genistin of four kinds of clear creams, jateorrhizine, palmatine, jamaicin, Z- Ligustilide and the Z-3- butylidene phthalide of S4
Content reach the ranges of needs.
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| PCT/CN2020/072103 WO2020098831A1 (en) | 2018-11-14 | 2020-01-14 | Gynecological qianjin capsule and quality control method therefor |
| US17/293,920 US12144841B2 (en) | 2018-11-14 | 2020-01-14 | Fuke Qianjin Capsule and quality control method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1298730A (en) * | 1999-12-07 | 2001-06-13 | 株洲千金药业股份有限公司 | Process for preparing 'Qianjin' capsule to treat genopathy |
| CN1733105A (en) * | 2005-08-18 | 2006-02-15 | 贵阳云岩西创药物科技开发有限公司 | Preparation for treating gynecological disease, its preparation process and quality control method |
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| CN106950309A (en) * | 2017-03-30 | 2017-07-14 | 南京中医药大学 | Not same amount than Radix Angelicae Sinensis and safflower medicine pair method of quality control |
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