CN109106786A - A method of improving FUKE QIANJIN PIAN disintegration time limited - Google Patents

A method of improving FUKE QIANJIN PIAN disintegration time limited Download PDF

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Publication number
CN109106786A
CN109106786A CN201811342270.5A CN201811342270A CN109106786A CN 109106786 A CN109106786 A CN 109106786A CN 201811342270 A CN201811342270 A CN 201811342270A CN 109106786 A CN109106786 A CN 109106786A
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fuke qianjin
qianjin pian
content
less
andrographolide
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龚云
张鹏
李伏君
彭开锋
凌勇根
白璐
袁红波
何娟娟
赵威
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Zhuzhou Qianjin Pharmaceutical Co Ltd
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Zhuzhou Qianjin Pharmaceutical Co Ltd
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Abstract

The invention discloses a kind of methods for improving FUKE QIANJIN PIAN disintegration time limited.The FUKE QIANJIN PIAN is made using philippine flemingia root, leatherleaf mahonia, Herba Andrographitis, single side needle, Caulis Spatholobi, Radix Angelicae Sinensis, Radix Codonopsis, cherokee rose root by raw material, in the preparation process of FUKE QIANJIN PIAN, the total amount of the content of Z-3- butylidene phthalide, andrographolide and Dehydro and drographolide is regulated and controled, the content of Z-3- butylidene phthalide is no less than 0.015mg in the every FUKE QIANJIN PIAN, and the total amount of andrographolide and Dehydro and drographolide is no less than 1.1mg；It is preferred that the detection of the content uses HPLC method.The present invention specifies that the content of Z-3- butylidene phthalide and the content of andrographolide and Dehydro and drographolide act on the great influence of properties of product and make accurate restriction in FUKE QIANJIN PIAN, compared to existing FUKE QIANJIN PIAN, its disintegration time limited makes moderate progress, effective component release is fast, rapid-action, and clinical efficacy has further raising.

Description

A method of improving FUKE QIANJIN PIAN disintegration time limited
Technical field
The present invention relates to technical field of traditional Chinese medicines, and in particular, to a method of improve FUKE QIANJIN PIAN disintegration time limited.
Background technique
FUKE QIANJIN PIAN is by philippine flemingia root, cherokee rose root, Herba Andrographitis, leatherleaf mahonia, single side needle, Radix Angelicae Sinensis, Caulis Spatholobi, 8 taste of Radix Codonopsis Drug made of 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 leukorrhagia Amount is more, color Huang matter is thick, smelly dirty, underbelly pain, waist sacrum ache, spiritlessness and weakness；Chronic pelvic inflammatory disease, endometritis, chronic uterine neck Inflammation is shown in above-mentioned patient.
In existing Chinese Pharmacopoeia, the content of FUKE QIANJIN PIAN is identified, is only to define wherein andrographolide Contain Herba Andrographitis specifically in every with the total content of Dehydro and drographolide with andrographolide (C20H30O5) and dehydration wear Heart lotus lactone (C20H28O4) total amount meter, 0.8mg must not be less than.And in the compatibility ingredient of FUKE QIANJIN PIAN, Herba Andrographitis is only As ministerial drug therein.Obviously, existing standard does not carry out correlative study and regulation to the other compositions in a thousand pieces of gold piece.This Shen It asks someone to find that other effective components in FUKE QIANJIN PIAN may will affect effective component by long-term a large amount of experimental summary Release, to influence the clinical efficacy of FUKE QIANJIN PIAN.It is studied based on the present invention, it is necessary to propose a kind of new solution technical side Case promotes the existing quality for having FUKE QIANJIN PIAN product on the market, further to improve controlling for FUKE QIANJIN PIAN Therapeutic effect.
Summary of the invention
The purpose of the invention is to overcome the above-mentioned deficiency of the prior art, when a kind of disintegration of improvement FUKE QIANJIN PIAN is provided The method of limit passes through the content and andrographolide of science restriction Z-3- butylidene phthalide and containing for Dehydro and drographolide Amount, can effectively improve FUKE QIANJIN PIAN disintegration time limited, so that effective component release is fast, rapid-action, improve facing for FUKE QIANJIN PIAN Bed curative effect.
To achieve the goals above, the present invention is achieved by following scheme:
A method of improving FUKE QIANJIN PIAN disintegration time limited, the FUKE QIANJIN PIAN is with philippine flemingia root, leatherleaf mahonia, punching Lotus, single side needle, Caulis Spatholobi, Radix Angelicae Sinensis, Radix Codonopsis, cherokee rose root are made of raw material, in the preparation process of FUKE QIANJIN PIAN, to Z-3- fourth The total amount of the content of alkenyl phthalide, andrographolide and Dehydro and drographolide is regulated and controled, in the every FUKE QIANJIN PIAN The content of Z-3- butylidene phthalide is no less than 0.015mg, and the total amount of andrographolide and Dehydro and drographolide is no less than 1.1mg；It is preferred that the detection of the content uses HPLC method.
Chinese medicine compound prescription is the organic whole having levels with structure, is not the simple adduction of each simple, the present invention Chinese medicine compound prescription is considered as an entirety, system research is carried out to its chemical component, inherently illustrates the substance of compound pharmacological action Basis, and foundation is provided for the control of the quality standard of compound.Radix Angelicae Sinensis is the adjutant simply in FUKE QIANJIN PIAN, Z-3- cyclobutenyl benzene Phthalein derives from Radix Angelicae Sinensis, inventors have found that the content of Z-3- butylidene phthalide has a major impact the disintegration time limited of FUKE QIANJIN PIAN. When handle in every FUKE QIANJIN PIAN (being reference by existing product and production target, the quality of every FUKE QIANJIN PIAN is 320mg) The content of Z-3- butylidene phthalide is controlled in 0.015mg or more, and prepared FUKE QIANJIN PIAN compared with the prior art, is disintegrated Time limit is shorter, and effective component release is fast, rapid-action, and clinical therapeutic efficacy is made to get a promotion.
Preferably, the content of Z-3- butylidene phthalide is no less than 0.02mg in the every FUKE QIANJIN PIAN, in Herba Andrographitis The total amount of ester and Dehydro and drographolide is no less than 1.4mg；It is preferred that the detection of the content uses HPLC method.
It is highly preferred that the content of Z-3- butylidene phthalide is 0.04~0.08mg, punching in the every FUKE QIANJIN PIAN The total amount of lotus lactone and Dehydro and drographolide is no less than 1.93mg；It is preferred that the detection of the content uses HPLC method.
Preferably, the sample of the HPLC method detection is prepared through following method:
10 FUKE QIANJIN PIANs are taken to remove coating, it is accurately weighed, it is finely ground, 0.3g is taken, is set in container, methanol is added in precision 20mL, weighing, is ultrasonically treated 15min at power 200W, frequency 40kHz, is down to room temperature, weighs, supplies less loss with methanol Weight shakes up, filtration, obtains detection liquid.
Preferably, the condition of the HPLC method detection is as follows:
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 30 DEG C as B phase, gradient elution, flow velocity 1.0mL/min, Detection wavelength 254nm, column temperature, into Sample amount is 10 μ L.
Preferably, the preparation method of the FUKE QIANJIN PIAN includes the following steps:
Using philippine flemingia root, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as compatibility；
S1. Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis are chosen, the fine powder of 100 mesh or more is ground into, is stayed by at least 93.3% powder rate that obtains It takes spare；
S2. selection single side needle and cherokee rose root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root, extracting in water 2 times, each extraction time It is 2 hours, Extracting temperature is 85~95 DEG C, filters to take filtrate, filtrate is condensed into the clear cream of 1.08/85 DEG C of CF；
S3. the clear cream of the fine powder of S1 and S2 are mixed, and carries out HPLC method detection, control Z-3- fourth in every milligram of mixture The total amount that the content of alkenyl phthalide is no less than 0.00008mg, andrographolide and Dehydro and drographolide is no less than 0.00619mg；Then it dries, tabletting, package piece obtain the FUKE QIANJIN PIAN.
As a kind of selectable specific embodiment, the preparation method of the FUKE QIANJIN PIAN includes the following steps:
Using philippine flemingia root, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as compatibility, wherein when Return, the dosage of Radix Codonopsis, Herba Andrographitis and single side needle is respectively the 9% of medicinal material total amount；Cherokee rose root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root Dosage is respectively the 16% of medicinal material total amount；
S1. Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis are chosen, the fine powder of 100 mesh or more is ground into, is stayed by at least 93.3% powder rate that obtains It takes spare；
S2. single side needle and cherokee rose root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root are chosen, extracting in water 2 times, adds the five tastes for the first time The water of 12 times of Chinese medicine total weight amounts, the water of second plus 10 times of traditional Chinese medicine of the five flavours total weight amount, each extraction time are 2 hours, are mentioned Taking temperature is 95 DEG C, filters to take filtrate, filtrate is condensed into the clear cream of 1.08/85 DEG C of CF；
S3. the clear cream of the fine powder of S1 and S2 are mixed, and carries out HPLC method detection, control Z-3- fourth in every milligram of mixture The total amount that the content of alkenyl phthalide is no less than 0.00008mg, andrographolide and Dehydro and drographolide is no less than 0.00619mg；Then it dries, tabletting, package piece obtain the FUKE QIANJIN PIAN.
It is highly preferred that the content of Z-3- butylidene phthalide described in step S3 is no less than 0.00011mg, andrographolide and takes off The total amount of water andrographolide is no less than 0.00788mg.
It is highly preferred that the content of Z-3- butylidene phthalide described in step S3 is 0.00023~0.00045mg, in Herba Andrographitis The total amount of ester and Dehydro and drographolide is no less than 0.01086mg.
Preferably, the preparation process of HPLC method test sample described in step S3 are as follows: take 0.3g clear cream and fine powder mixture 75% methanol aqueous solution of 200mL is added to dissolve, weighing, then ultrasound 15min, adds 75% methanol aqueous solution to supply after ultrasonic Then the weight of loss takes 2mL lysate to be diluted to 10mL with 75% methanol aqueous solution again, cross 0.45 μm of miillpore filter, take filter Liquid is as solution to be measured.
Preferably, the condition of the detection of HPLC method described in step S3 are as follows: use Kromasil 100-5-C18 chromatographic column (250mm × 4.6mm, 5 μm), mobile phase is using acetonitrile as A phase and 0.1% phosphate aqueous solution as B phase, gradient elution, flow velocity For 1.0mL/min, Detection wavelength 254nm, column temperature is 30 DEG C, and sample volume is 10 μ L.
Compared with prior art, the invention has the following advantages:
The applicant has found that the other compositions in FUKE QIANJIN PIAN may will affect by long-term a large amount of experimental summary The release of ingredient is imitated, to influence the clinical efficacy of FUKE QIANJIN PIAN, based on present invention research, the present invention is in product preparation process In creatively increase quality inspection steps, by science limit Z-3- butylidene phthalide content and andrographolide with The content of Dehydro and drographolide can effectively improve FUKE QIANJIN PIAN disintegration time limited, so that effective component release is fast, rapid-action, Improve the clinical efficacy of FUKE QIANJIN PIAN.
The present invention passes through the analysis to chemical components a variety of in FUKE QIANJIN PIAN, it is expected to establish control FUKE QIANJIN PIAN quality New standard, for the standard on existing standards of pharmacopoeia, science increases the core component Z-3- butylidene phthalide in crude drug Content limits, according to FUKE QIANJIN PIAN made of the range criterion, compared to the prior art, it is ensured that product disintegration time limited is more Short, effective component release is fast, rapid-action, and clinical efficacy has further raising.
Meanwhile the present invention further provides content detection is carried out using HPLC method, not only testing result accuracy is high, inspection Survey process is quick, easy, is preferably applied in the actual production process of FUKE QIANJIN PIAN of the present invention, in original preparation The content that can detect and monitor simultaneously plurality of active ingredients in technique, is conducive to establish new quality testing 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.Embodiment 1 FUKE QIANJIN PIAN
FUKE QIANJIN PIAN is prepared using following methods:
The formula of FUKE QIANJIN PIAN: Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis and single side needle dosage be respectively the 9% of medicinal material total amount；Jin Ying Root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root dosage be respectively the 16% of medicinal material total amount.
1, Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis are chosen, the fine powder of 100 mesh or more is ground into, is left and taken by at least 93.3% powder rate that obtains It is spare；
2, single side needle and cherokee rose root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root are chosen, extracting in water 2 times, is added in the five tastes for the first time The water of 12 times of medicine total weight amounts, the water of second plus 10 times of traditional Chinese medicine of the five flavours total weight amount, each extraction time are 2 hours, are extracted Temperature is 95 DEG C, filters to take filtrate, filtrate is condensed into the clear cream of 1.08/85 DEG C of CF；
3, the clear cream of the fine powder of step 1 and step 2 is mixed, and carries out HPLC method detection, controlled in every milligram of mixture The total amount that the content of Z-3- butylidene phthalide is no less than 0.00008mg, andrographolide and Dehydro and drographolide is no less than 0.00619mg；Then it dries, tabletting, package piece, obtains the FUKE QIANJIN PIAN (320mg/ piece).
When testing result is unsatisfactory for above-mentioned condition, it is substandard product, finished product is not made.
FUKE QIANJIN PIAN is prepared referring to the above method, the product of 10 batches is randomly selected from long-term, a large amount of product, And the detection of HPLC method is carried out to the FUKE QIANJIN PIAN product of each batch preparation:
(1) preparation of liquid is detected
It randomly selects with a batch of FUKE QIANJIN PIAN 10 (320mg/ piece), removes coating, it is accurately weighed, it is finely ground, it takes 0.3g is set in container, and methanol 20mL is added in precision, and weighing is ultrasonically treated 15min at power 200W, frequency 40kHz, is down to Room temperature, weighing, the weight of less loss is supplied with methanol, is shaken up, and is filtered, and detection liquid is obtained.
(2) HPLC method detects
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 30 DEG C as B phase, gradient elution, flow velocity 1.0mL/min, Detection wavelength 254nm, column temperature, into Sample amount is 10 μ L.
(3) testing result
Testing result is as shown in table 1.
Three kinds of component contents (μ g/ piece) in the FUKE QIANJIN PIAN of the different batches of 1 embodiment 1 of table preparation
Z-3- butylidene phthalide μ g Andrographolide μ g Dehydro and drographolide μ g
Batch 1 16.42±0.99 608.24±0.34 503.87±0.45
Batch 2 17.80±1.04 669.26±0.55 541.96±0.97
Batch 3 21.21±0.09 670.44±0.29 565.82±2.53
Batch 4 23.53±0.74 675.18±5.98 575.13±0.89
Batch 5 23.61±0.14 721.40±0.07 594.14±0.22
Batch 6 26.10±0.38 786.11±0.19 595.60±10.40
Batch 7 26.14±3.85 796.13±0.92 596.38±0.99
Batch 8 27.23±0.97 898.70±11.08 605.69±0.39
Batch 9 40.39±0.80 1132.64±0.69 612.54±3.97
Batch 10 47.85±0.13 1242.40±0.75 641.33±0.04
1 FUKE QIANJIN PIAN of comparative example
The substandard product in embodiment 1 is chosen, is directly spray-dried, then pelletizes, is canned, obtaining the gynaecology A thousand pieces of gold piece, the regulation of 2015 editions Pharmacopoeias of the People's Republic of China, the content of every FUKE QIANJIN PIAN are 0.32g.And to each The FUKE QIANJIN PIAN product of batch carries out HPLC detection using identical method.And according to Pharmacopoeia of the People's Republic of China woman The requirement of section's a thousand pieces of gold piece is detected, and in every FUKE QIANJIN PIAN, the total amount of andrographolide and Dehydro and drographolide is greater than 0.8mg, it is consistent with commercially available gynaecology's FUKE QIANJIN PIAN.Testing result is as shown in table 2.
Three kinds of component contents (μ g/ piece) in the FUKE QIANJIN PIAN of the different batches of 2 comparative example 1 of table preparation
Z-3- butylidene phthalide μ g Andrographolide μ g Dehydro and drographolide μ g
Batch 1 (comparison) 12.4±1.8 507.56±0.75 435.94±5.45
Batch 2 (comparison) 12.44±0.74 524.85±3.54 445.94±0.3
Batch 3 (comparison) 12.72±6.97 539.41±1.21 459.41±12.74
Batch 4 (comparison) 13.63±0.45 572.22±0.42 480.16±0.28
Batch 5 (comparison) 14.13±5.85 586.42±0.27 488.94±0.49
The detection of 1 FUKE QIANJIN PIAN disintegration time limited of application examples
Disintegration time limited detection, disintegration time mensuration are carried out to the finished product of 1 batch 1~10 of embodiment, comparative example batch 1~5 Method detection method is shown in Table 3 referring to " Chinese Pharmacopoeia " 2015 editions tablet disintegration time limit inspection techniques, specific test result.
The disintegration time limited of 1 different batches FUKE QIANJIN PIAN of 3 embodiment 1 of table and comparative example
Appearance character Friability Hardness Disintegration time limited
1 batch 1 of embodiment It is qualified It is qualified It is qualified 25min12s
1 batch 2 of embodiment It is qualified It is qualified It is qualified 24min50s
1 batch 3 of embodiment It is qualified It is qualified It is qualified 24min15s
1 batch 4 of embodiment It is qualified It is qualified It is qualified 23min19s
1 batch 5 of embodiment It is qualified It is qualified It is qualified 22min30s
1 batch 6 of embodiment It is qualified It is qualified It is qualified 21min50s
1 batch 7 of embodiment It is qualified It is qualified It is qualified 20min21s
1 batch 8 of embodiment It is qualified It is qualified It is qualified 19min20s
1 batch 9 of embodiment It is qualified It is qualified It is qualified 19min2s
1 batch 10 of embodiment It is qualified It is qualified It is qualified 18min42s
1 batch 1 of comparative example It is qualified It is qualified It is qualified 32min52s
1 batch 2 of comparative example It is qualified It is qualified It is qualified 32min32s
1 batch 3 of comparative example It is qualified It is qualified It is qualified 32min10s
1 batch 4 of comparative example It is qualified It is qualified It is qualified 31min29s
1 batch 5 of comparative example It is qualified It is qualified It is qualified 30min26s
As seen from the results in Table 3, the disintegration time limited of FUKE QIANJIN PIAN obtained by 1 each batch of the embodiment of the present invention is compared to right 1 each batch FUKE QIANJIN PIAN of ratio be improved significantly, the release of effective component is fast, rapid-action, be conducive to improve clinical treatment Effect.
2 result in clinical application of application examples
In order to FUKE QIANJIN PIAN more provided by the present invention and original method preparation FUKE QIANJIN PIAN drug effect whether It has differences, has carried out clinical test.Each testing site is centralized and unified according to the requirement in relation to new drug research, has drafted clinical research Principle establishes diagnostic criteria, is included in standard, dumping standard, and as criterion, collects observation case.Simultaneously in use In accordance with the method for administration of specification appended by drug, start to take medicine when medical, 7 days as one therapeutic course, two courses for the treatment of of continuous use, and press The clinical observation table drafted collects clinical symptoms and Signs variation.
One, chronic pelvic inflammatory disease
Table 4 is the second affiliated hospital of Hunan College of Traditional Chinese Medicine, the academy of traditional Chinese medicine of Hunan Province, attached hospital of Hunan Medical University etc. Using the drug, suffers from undergoing chronic pelvic inflammation to 120 and takes the clinical change after two courses for the treatment of of FUKE QIANJIN PIAN and count, It is divided into 3 groups, every group of 40 patients.Concrete outcome is shown in Table 4.
4 undergoing chronic pelvic inflammation of table treats improvement situation and proportion table
Two, chronic appendages inflammation
Clinical change after 120 chronic appendages inflammation patients are taken with two courses for the treatment of of FUKE QIANJIN PIAN counts, and is divided into 3 Group, every group of 40 patients.Concrete outcome is shown in Table 5~7.Wherein, table 5 is 120 chronic appendages inflammation patient's gynecologial examination situations, table 6 take curative effect statistical result after FUKE QIANJIN PIAN for chronic appendages inflammation patient, and table 7 is that chronic appendages inflammation patient takes gynaecology's a thousand pieces of gold The change situation of symptom before and after piece.
5 gynecologial examination situation of table
Position Number of cases Obvious tenderness General tenderness Light tenderness
Side adnexitis 78 27 30 21
Bilateral adnexitis 42 18 12 12
It is total 120 45 42 33
Table 6 takes the curative effect after FUKE QIANJIN PIAN
7 chronic appendages inflammation patient of table takes the change of symptom before and after FUKE QIANJIN PIAN
Three, endometritis
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.120 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.The FUKE QIANJIN PIAN of 1 batch 1 of embodiment is given on the basis of blank control group by observation group, and control group is in sky 1 batch 1 of comparative example is given on the basis of white control group, FUKE QIANJIN PIAN prepared by batch 5.See Table 8 for details for treatment results~and 10.
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.
8 Clinical efficacy comparison of table
Batch (number of cases) It is effective Effectively In vain Obvious effective rate It is efficient
1 batch 1 (30) of embodiment 25 4 1 83.33% 96.67%
1 batch 1 (30) of comparative example 20 5 5 66.67% 83.33%
1 batch 5 (30) of comparative example 22 6 2 73.33% 93.33%
Blank control group (30) 15 8 7 50.00% 76.67%
The recovered situation of table September compares
10 ultrasound diagnosis of table recovery is compared
By 8~10 result of table it is found that compared to the FUKE QIANJIN PIAN for only controlling Herba Andrographitis effective component originally, the present invention is same When control Z-3- butylidene phthalide, andrographolide and Determination of Dehydroandrographoliin FUKE QIANJIN PIAN, improve gynaecology thousand Gold plaque treats the effect of endometritis, is embodied in efficient and obvious effective rate and gets a promotion, and illustrates in control Z-3- butylene When base phthalide, andrographolide and Determination of Dehydroandrographoliin, FUKE QIANJIN PIAN can have preferably with antibiotic and progestational hormone Mutual cooperation effect.
To sum up, 1 each batch FUKE QIANJIN PIAN of the embodiment of the present invention is in treatment chronic pelvic inflammatory disease, chronic appendages inflammation and intrauterine The effect of the scorching aspect of film is superior to the FUKE QIANJIN PIAN of 1 different batches of comparative example.In process of production, increase to fine powder and clear cream The detection of mixture effective component controls the content of 3 kinds of effective component in the FUKE QIANJIN PIAN obtained in a certain zone of reasonableness It is interior, the disintegration time limited of finished product is effectively improved, the rate of release of effective component is improved, so that finished product is in chronic pelvic inflammatory disease, slow The clinical therapeutic efficacy of property adnexitis and endometritis is effectively promoted.
To sum up, in process of production, increase the detection to fine powder and clear cream mixture effective component, make the gynaecology thousand obtained The content of 3 kinds of effective component controls in a certain zone of reasonableness in gold plaque, and the disintegration time limited of product obtained in this way obtains effectively Improve, is conducive to the rate of release for improving effective component, and then promote clinical therapeutic efficacy.
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. it is a kind of improve FUKE QIANJIN PIAN disintegration time limited method, the FUKE QIANJIN PIAN with philippine flemingia root, leatherleaf mahonia, Herba Andrographitis, Single side needle, Caulis Spatholobi, Radix Angelicae Sinensis, Radix Codonopsis, cherokee rose root are made of raw material, which is characterized in that in the preparation process of FUKE QIANJIN PIAN, The total amount of the content of Z-3- butylidene phthalide, andrographolide and Dehydro and drographolide is regulated and controled, the every gynaecology The content of Z-3- butylidene phthalide is no less than 0.015mg in a thousand pieces of gold piece, and the total amount of andrographolide and Dehydro and drographolide is not Less than 1.1mg；It is preferred that the detection of the content uses HPLC method.
2. method according to claim 1, which is characterized in that Z-3- butylidene phthalide contains in the every FUKE QIANJIN PIAN The total amount of amount no less than 0.02mg, andrographolide and Dehydro and drographolide is no less than 1.4mg；It is preferred that the detection of the content Using HPLC method.
3. method according to claim 2, which is characterized in that Z-3- butylidene phthalide contains in the every FUKE QIANJIN PIAN Measuring is 0.04~0.08mg, and the total amount of andrographolide and Dehydro and drographolide is no less than 1.93mg；It is preferred that the content Detection uses HPLC method.
4. method according to any one of the claim 1 to 3, which is characterized in that the sample of the HPLC method detection passes through such as lower section Method preparation:
10 FUKE QIANJIN PIANs are taken to remove coating, it is accurately weighed, it is finely ground, 0.3g is taken, is set in container, methanol 20mL is added in precision, Weighing, is ultrasonically treated 15min at power 200W, frequency 40kHz, is down to room temperature, weighs, the weight of less loss is supplied with methanol, It shakes up, filters, obtain detection liquid.
5. method according to any one of the claim 1 to 3, which is characterized in that the condition of the HPLC method detection is as follows:
Using Kromasil 100-5-C18 chromatographic column (250mm × 4.6mm, 5 μm), mobile phase is using acetonitrile as A phase and 0.1% Phosphate aqueous solution is 30 DEG C as B phase, gradient elution, flow velocity 1.0mL/min, Detection wavelength 254nm, column temperature, sample volume For 10 μ L.
6. method according to any one of the claim 1 to 3, which is characterized in that the preparation method of the FUKE QIANJIN PIAN includes Following steps:
Using philippine flemingia root, cherokee rose root, Herba Andrographitis, Radix Angelicae Sinensis, leatherleaf mahonia, single side needle, Caulis Spatholobi and Radix Codonopsis as compatibility；
S1. choose Radix Angelicae Sinensis, Radix Codonopsis, Herba Andrographitis, be ground into the fine powder of 100 mesh or more, by least 93.3% powder rate leave and take it is standby With；
S2. single side needle and cherokee rose root, Caulis Spatholobi, leatherleaf mahonia and philippine flemingia root are chosen, extracting in water 2 times, each extraction time is 2 small When, Extracting temperature is 85~95 DEG C, filters to take filtrate, filtrate is condensed into the clear cream of 1.08/85 DEG C of CF；
S3. the clear cream of the fine powder of S1 and S2 are mixed, and carries out HPLC method detection, control Z-3- cyclobutenyl in every milligram of mixture The total amount that the content of phthalide is no less than 0.00008mg, andrographolide and Dehydro and drographolide is no less than 0.00619mg；So After dry, tabletting, package piece obtain the FUKE QIANJIN PIAN.
7. method according to claim 6, which is characterized in that the content of Z-3- butylidene phthalide described in step S3 is no less than The total amount of 0.00011mg, andrographolide and Dehydro and drographolide are no less than 0.00788mg.
8. method according to claim 7, which is characterized in that the content of Z-3- butylidene phthalide described in step S3 is The total amount of 0.00023~0.00045mg, andrographolide and Dehydro and drographolide are no less than 0.01086mg.
9. method according to claim 6, which is characterized in that the preparation process of HPLC method test sample described in step S3 Are as follows: take 0.3g clear cream and fine powder mixture that 75% methanol aqueous solution of 200mL is added to dissolve, weighing, then ultrasound 15min, ultrasound are tied 75% methanol aqueous solution of Shu Houjia supplies the weight of loss, then 2mL lysate is taken to be diluted to 10mL with 75% methanol aqueous solution again, 0.45 μm of miillpore filter is crossed, takes filtrate as solution to be measured.
10. method according to claim 6, which is characterized in that the condition of the detection of HPLC method described in step S3 are as follows: use Kromasil 100-5-C18 chromatographic column (250mm × 4.6mm, 5 μm), mobile phase are water-soluble using acetonitrile as A phase and 0.1% phosphoric acid Liquid is 30 DEG C as B phase, gradient elution, flow velocity 1.0mL/min, Detection wavelength 254nm, column temperature, and sample volume is 10 μ L.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1251763A (en) * 1998-10-21 2000-05-03 株洲千金药业股份公司 Process for preparing Chinese medicine 'Qianjin tablets' for treating gynopathy

Patent Citations (1)

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CN1251763A (en) * 1998-10-21 2000-05-03 株洲千金药业股份公司 Process for preparing Chinese medicine 'Qianjin tablets' for treating gynopathy

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