CN1273115A

CN1273115A - Process for refining injection 'Shuanghuanglian'

Info

Publication number: CN1273115A
Application number: CN 99106224
Authority: CN
Inventors: 盖兆光; 梁起臣
Original assignee: Individual
Current assignee: Individual
Priority date: 1999-05-05
Filing date: 1999-05-05
Publication date: 2000-11-15
Anticipated expiration: 2019-05-05
Also published as: CN1095364C

Abstract

A refined injection "Shuanghuanglian" is prepared through decocting honeysuckle flower and forsythia fruit; concentrating the filtrate then adding alcohol; laying the solution aside; recovering alcohol, adding deionized water, regulating pH value; laying aside, filtering with ultrafiltrating membrane, concentrating; adding alcohol to concentrated liquid; laying aside, recovering alcohol; filtering to obtain extract; mixing with the obtained baicalin powder and water for injection, boiling and filtering with micropore filter membrane to obtain the product. Its advantages are short preparing period, low cost, high transparency and low tannin content.

Description

A kind of production technology of refining injection ' Shuanghuanglian '

The present invention relates to field of medicine preparations, particularly the production technology of refining injection ' Shuanghuanglian '.

Radix Scutellariae is the Labiatae perennial vertical herbage, has effects such as antibiotic, analgesic, blood pressure lowering.

Flos Lonicerae is Radix Ophiopogonis, is the perennial half evergreen voluble shrub of Caprifoliaceae, and its flower and stem have the effect of heat-clearing and toxic substances removing.

Fructus Forsythiae is the machaka of Oleaceae, has the effect of heat-clearing and toxic substances removing, detumescence, eliminating stagnation.

In recent decades, owing to use antibiotic in a large number repeatedly for a long time, Resistant strain increases gradually, and some antibiotic also has certain toxic and side effects, by Radix Scutellariae, Flos Lonicerae and Fructus Forsythiae three flavor medicines is that the medicament SHUANGHUANLIAN of raw material production belongs to pure Chinese medicinal preparation, have relieving exterior-interior syndrome, the effect of clearing away heat in both QI and blood is used for affection due to external wind and heat, epidemic febrile disease, has good heat-clearing toxin-expelling functions, not only toxicity is low, and the effective percentage of upper respiratory tract infection and viral pneumonia is reached 92%, and cure rate reaches 81%.

At present the process cycle of production SHUANGHUANGLIAN ZHUSHEYE is longer, and production cost is higher, and technology stability and shelf-life be still waiting to improve, the color and luster of injection and when causing patient infusion the content of tannin of pain also need further to reduce.

The purpose of this invention is to provide a kind of production long shelf-life, clarity height, the production technology of the SHUANGHUANGLIAN ZHUSHEYE that content of tannin is low.

For achieving the above object, the present invention takes following design: a kind of technology of producing refining injection ' Shuanghuanglian ' may further comprise the steps:

(1) be that the Flos Lonicerae of 0.8-1.2: 0.8-1.2 and the Fructus Forsythiae crude drug back that is soaked in water decocts each 1-2 hour 2 times with weight ratio;

(2) decoct the merging of gained filtrate with above-mentioned twice, concentrate the back and add ethanol, make that ethanol content is 75%-85% in the solution;

(3) above-mentioned solution leaves standstill 12-24 hour after-filtration under 0 ℃ of-5 ℃ of condition, reclaims supernatant;

(4) ethanol in the above-mentioned gained supernatant is recycled after, add the long-pending 3-4 of solution body deionized water doubly, and transfer pH to 5.0-7.0;

(5) gained solution left standstill 24-48 hour, microporous filter membrane leaching supernatant concentrated;

(6) in above-mentioned concentrated solution, add ethanol, make that concentration of ethanol is 70%-85% in the solution;

(7) gained solution recycles the ethanol in the solution after leaving standstill 12-24 hour under 0 ℃ of-5 ℃ of condition;

(8) with after the filtration of gained solution, obtain extractum;

(9) baicalin powder that above-mentioned extractum, conventional method are obtained and water for injection are the mixed of 0.8-1.2: 1.8-2.2: 800-1200 with the weight ratio, heated and boiled 15-20 minute;

(10) carry out filtering with microporous membrane after the cooling, filtrate fill sterilization obtains SHUANGHUANGLIAN ZHUSHEYE.

The present invention is owing to adopted above-mentioned design, production cycle to shorten, and cost reduces; Owing to adopted repeatedly filter press, ultrafiltration membrance filter and heat treatment refrigeration precipitated impurities, macromole pigment and content of tannin in the injection are descended significantly, the clarity of injection is than descended two colors number of existing product, the content of tannin drops to 0.8-1.0% by original about 2%, and the pain when removing patient infusion will play an important role; The quality standard standardization comes control of quality with assay, thereby makes technology stability that large increase arranged in the production process of the present invention, and the maintenance phase of product has been brought up to 2 years by original 1 year.

Acute toxicity test shows that this product is nontoxic, gives no death and poisoning symptom in mice lavage and the lumbar injection seven days with Cmax and maximum volume; Pharmacodynamic test of active extract shows that this product has analgesic and antiphlogistic effect; Resist bacteriostatic test in the external and body and show, this product is to Diplococcus pneumoniae, staphylococcus aureus, and Bacillus typhi paid by the first type and indoor dysentery bacterium has inhibitory action, body temperature and cell rising state when having improved inflammation simultaneously; Antivirus test shows has the obvious suppression effect to respiratory tract pulmonary antibacterial, virus and influenza virus.

The invention will be further described below in conjunction with specific embodiment.

Embodiment 1:

Certainly put forward baicalin powder production SHUANGHUANGLIAN ZHUSHEYE with conventional method

One, the extraction of baicalin powder.

1, gets 2kg Radix Scutellariae crude drug and add suitable quantity of water immersion back decoction 2 times, each 2 hours;

2, decoct gained solution plate-and-frame filtration with above-mentioned twice after, merging filtrate is with 2 mol HCL accent pH to 1.5, leave standstill 24 hours after, carry out plate-and-frame filtration again one time;

3, with adding the deionized water of 8 times of filtrate volumes in the gained filtrate, behind 40% NaOH adjust pH 7.0, add 95% ethanol, make that alcoholic acid content is 75% in the solution; Left standstill 24 hours;

4, supernatant is used the polyamide filtering with microporous membrane, gained filtrate is transferred pH to 2.0 with 2 mol HCL, and 40 ℃ of insulations are after 20 minutes, 0.65 micron polyamide filtering with microporous membrane of reuse;

5, add 95% ethanol in filtrate, alcoholic acid content is 75% to the filtrate; Behind 40% NaOH conciliation pH to 4.0, add the deionized water of long-pending 10 times of solution body; Reuse 40% NaOH transfers pH to 6.0;

6, in solution, add 0.5% active carbon, left standstill 12 hours, filter decarburization;

7, take off ethanol with ethanol backwater tower after, with solution concentration, drying under reduced pressure obtains 40 gram baicalin powder;

Two, the preparation of Flos Lonicerae, Fructus Forsythiae extractum

1, extracting honeysuckle, each 2kg of Fructus Forsythiae crude drug soak the back with suitable quantity of water and decoct each 2 hours 2 times;

2, merge after will be above-mentioned decocting gained solution filter press twice, it is 1.25 (75 ℃) that heating is concentrated into proportion, adds 95% ethanol, makes that ethanol content is 75% in the solution;

3, with above-mentioned solution after leaving standstill 24 hours under 0 ℃ of condition, filter press reclaims supernatant;

4, the ethanol in the supernatant is reclaimed with alcohol distillation column, add the deionized water of long-pending 3 times of solution body, pH is transferred to 7.0 with 40% NaOH;

5, the gained solution left standstill is 48 hours, 0.25 micron polyamide microporous filter membrane leaching supernatant, and it is 1.15 (75 ℃) that heating is concentrated into proportion;

6, in above-mentioned concentrated solution, add 95% ethanol, make that concentration of alcohol is 75% in the solution;

7, solution was left standstill 24 hours under 0 ℃ of condition, ethanol is recycled with alcohol distillation column;

8, will obtain extractum 80g behind the gained solution filter press;

Three, the preparation of SHUANGHUANGLIAN ZHUSHEYE:

1, with gained baicalin powder, extractum and water for injection weight ratio Hybrid Heating, boiled 20 minutes by 2.2: 1.2: 1200;

2, carry out the polyamide ultrafiltration membrance filter after the cooling, filtrate fill sterilization promptly obtains SHUANGHUANGLIAN ZHUSHEYE.

Embodiment 2

With commercially available baicalin powder production SHUANGHUANGLIAN ZHUSHEYE.

One, the preparation of Flos Lonicerae, Fructus Forsythiae extractum

1, extracting honeysuckle, each 2kg of Fructus Forsythiae crude drug soak the back with suitable quantity of water and decoct each 1 hour 2 times;

2, merge after will be above-mentioned decocting gained solution filter press twice, it is 1.20 (75 ℃) that heating is concentrated into proportion, adds 95% ethanol, makes that ethanol content is 70% in the solution;

3, with above-mentioned solution after leaving standstill 12 hours under 5 ℃ of conditions, filter press reclaims supernatant;

4, the ethanol in the supernatant is reclaimed with alcohol distillation column, add the deionized water of long-pending 4 times of solution body, pH is transferred to 5.0 with 40% NaOH;

5, the gained solution left standstill is 24 hours, 0.45 micron polyamide microporous filter membrane leaching supernatant, and it is 1.10 (75 ℃) that heating is concentrated into proportion;

6, in above-mentioned concentrated solution, add 95% ethanol, make that concentration of alcohol is 70% in the solution;

7, solution was left standstill 12 hours under 5 ℃ of conditions, ethanol is recycled with alcohol distillation column;

8, will obtain extractum 80g behind the gained solution filter press;

Two, the preparation of SHUANGHUANGLIAN ZHUSHEYE:

1, with commercially available baicalin powder, extractum and water for injection weight ratio Hybrid Heating, boiled 20 minutes by 1: 2: 1000;

Embodiment 3

One, the preparation of Flos Lonicerae, Fructus Forsythiae extractum

1, extracting honeysuckle, each 2kg of Fructus Forsythiae crude drug soak the back with suitable quantity of water and decoct each 1.5 hours 2 times;

2, merge after will be above-mentioned decocting gained solution filter press twice, it is 1.23 (75 ℃) that heating is concentrated into proportion, adds 95% ethanol, makes that ethanol content is 85% in the solution;

3, with above-mentioned solution after leaving standstill 20 hours under 3.3 ℃ of conditions, filter press reclaims supernatant;

4, the ethanol in the supernatant is reclaimed with alcohol distillation column, add the deionized water of long-pending 4 times of solution body, pH is transferred to 6.0 with 40% NaOH;

5, the gained solution left standstill is 20 hours, 0.8 micron polyamide microporous filter membrane leaching supernatant, and it is 1.13 (75 ℃) that heating is concentrated into proportion;

7, solution was left standstill 12 hours under 3 ℃ of conditions, ethanol is recycled with alcohol distillation column;

8, will obtain extractum 80g behind the gained solution filter press;

Two, the preparation of SHUANGHUANGLIAN ZHUSHEYE:

1, with commercially available baicalin powder, extractum and water for injection weight ratio Hybrid Heating, boiled 20 minutes by 0.9: 2.1: 1100;

Claims

1, a kind of technology of producing refining injection ' Shuanghuanglian ' is characterized in that: may further comprise the steps:

(8) with after the filtration of gained solution, obtain extractum;

2, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (2) step, concentrating the proportion of back solution under 70 ℃ of-80 ℃ of conditions is 1.2-1.25.

3, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (2) step, behind the adding ethanol, its concentration of ethanol is 75% in the solution.

4, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: reclaim ethanol with alcohol distillation column in described (4) step.

5, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: the microporous filter membrane in described (5) step is the polyamide membrane of 0.25-0.8 micron.

6, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (5) step, be 1.10-1.15 with proportion under ℃ of-80 ℃ conditions of solution concentration to 70 after the filtration.

7, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (6) step, behind the adding ethanol, the concentration of alcohol of solution is 75% in the solution.

8, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (7) step, reclaim the ethanol alcohol distillation column.

9, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: in described (9) step, the weight ratio of extractum, baicalin and water for injection is 1: 2: 1000.

10, the technology of production refining injection ' Shuanghuanglian ' according to claim 1 is characterized in that: the microporous filter membrane described in described (10) step is the polyamide membrane of 0.25-0.8 micron.