CN103948717B - A kind of Herba Hedyotidis Diffusae injection and its preparation method - Google Patents
A kind of Herba Hedyotidis Diffusae injection and its preparation method Download PDFInfo
- Publication number
- CN103948717B CN103948717B CN201410174335.5A CN201410174335A CN103948717B CN 103948717 B CN103948717 B CN 103948717B CN 201410174335 A CN201410174335 A CN 201410174335A CN 103948717 B CN103948717 B CN 103948717B
- Authority
- CN
- China
- Prior art keywords
- filtrate
- adjust
- solution
- filter
- filters
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention discloses a kind of Herba Hedyotidis Diffusae injection and its preparation method. This injection liquid is the sterile water solution that Spreading Hedyotis Herb is made through extracting, it is characterised in that: every ml soln is no less than 30 �� g containing 10-deacetyl asperulosidic acid methyl ester; Every ml soln is no less than 30 �� g containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside.
Description
Technical field
The present invention relates to the field of Chinese medicines, in particular to a kind of Herba Hedyotidis Diffusae injection and its preparation method.
Background technology
Herba Hedyotidis Diffusae injection records and becomes square preparation the 17 in the Sanitation Ministry medicine standard Chinese medicine, this product has clearing heat and detoxicating, inducing diuresis and reducing edema effect, the respiratory tract infection caused by poison is accumulate for damp and hot, tonsillitis, pneumonia, cholecystitis, ecphyaditis, carbuncle furuncle abscess and post-operative infection, also can be used for assistant treating cancer. Spreading Hedyotis Herb is mainly containing chemical compositions such as flavonoid, iridoids, anthracene quinone class and sterols, wherein flavones ingredient has inflammation antitumor, anti-oxidant, anti-, the effect such as antibacterial, for the main pharmacodynamics composition in Spreading Hedyotis Herb, discriminating item and the detected object of assay item in Herba Hedyotidis Diffusae injection ministerial standard are flavones ingredient. Commercially available Herba Hedyotidis Diffusae injection is the sterile water solution being made up through extracting of Spreading Hedyotis Herb, except containing except flavones ingredient, also containing a large amount of iridoid constituents. Now there are some researches show that part iridoid is inhibited to cells such as SMMC-7721, SW480, SW620, Be17402 and HepG2, also there is certain anti-tumor activity. Commercially available Herba Hedyotidis Diffusae injection adopts the preparation of stone sulphur method, and stone sulphur method obtains through refining the method that herbal injection belongs to conventional, has the features such as equipment is simple, processing ease, clarifying effect are good. But, applicant finds in Herba Hedyotidis Diffusae injection extracting process research process, and the stone sulphur method adopted at present can cause a large amount of losses of flavones ingredient, it is possible to can affect its clinical efficacy. Application number be 200510094404.2 patent " intravenous administered formulation of spreading hedyotis herb and its preparation method " disclose and adopt macroporous adsorbent resin and polymeric amide to go deimpurity method, the Herba Hedyotidis Diffusae injection that applicant adopts the method obtained detects through HPLC method, non-detection iridoid constituents acetyl woodruff acid methyl esters, the method can cause a large amount of losses of iridoid constituents as can be seen here, it is possible to can affect its anti-tumor activity.
Summary of the invention
It is an object of the invention to provide a kind of Herba Hedyotidis Diffusae injection and its preparation method, preparation method of the present invention is more scientific and reasonable, and drug quality is stablized, and compared with commercially available Herba Hedyotidis Diffusae injection, curative effect is better.
Herba Hedyotidis Diffusae injection provided by the invention, it is the sterile water solution being made up through extracting of Spreading Hedyotis Herb, and every ml soln is no less than 30 �� g containing 10-deacetyl asperulosidic acid methyl ester; Every ml soln is no less than 30 �� g containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside.
Herba Hedyotidis Diffusae injection provided by the invention, preparation method is as follows:
Get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, extracting solution concentrates in right amount, by milk of lime adjust ph to 7-10, or first by milk of lime adjust ph to 12, again by sulfur acid aqueous solution adjust ph to 7-10, refrigeration, filter, filtrate by sulfur acid aqueous solution adjust ph to 2-4, leave standstill, filter, filtrate adjust ph is to 5-7, adding ethanol makes alcohol content reach 65%��90%, refrigeration, filter, filtrate recycling ethanol also concentrates in right amount, add water to the 1-4 times amount of concentrated solution volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, obtain.
Herba Hedyotidis Diffusae injection provided by the invention, it is preferable that preparation method as follows:
Get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, extracting solution concentrates in right amount, by milk of lime adjust ph to 12, again by sulfur acid aqueous solution adjust ph to 7-8, refrigeration, filter, filtrate by sulfur acid aqueous solution adjust ph to 2-4, leave standstill, filter, filtrate adjust ph is to 5-7, adding ethanol makes alcohol content reach 65%��90%, refrigeration, filter, filtrate recycling ethanol also concentrates in right amount, add water to the 1-4 times amount of concentrated solution volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, obtain.
Herba Hedyotidis Diffusae injection provided by the invention, it is preferable that preparation method as follows:
Get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, extracting solution concentrates in right amount, by milk of lime adjust ph to 12, again by sulfur acid aqueous solution adjust ph to 7-8, refrigeration, filter, filtrate by sulfur acid aqueous solution adjust ph to 2-4, leave standstill, filter, filtrate adjust ph is to 5-7, adding ethanol makes alcohol content reach 75%��85%, refrigeration, filter, filtrate recycling ethanol also concentrates in right amount, add water to the 1-4 times amount of concentrated solution volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, obtain.
Herba Hedyotidis Diffusae injection provided by the invention, it is more preferable to preparation method as follows:
Get Spreading Hedyotis Herb 1000g, use 80% extraction using alcohol, extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 8, refrigerate 12-24 hour, filter, filtrate is by 50% sulphuric acid soln adjust ph to 3, leave standstill 12-24 hour, filter, filtrate by 40% sodium hydroxide solution adjust ph to 6.0-6.5, adding ethanol makes alcohol content reach 80%, refrigerate 24-72 hour, filter, filtrate recycling ethanol also concentrates to 250ml, add water to 500ml, add 0.5g-1.5g gac, stir even, filter, filtrate is with 40% sodium hydroxide solution adjust ph to 6.5��7.0, add 10g Polysorbate 80 and 1g sodium bisulfite, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, obtain.
The preparation method of ZHONGJIEFENG ZHUSHEYE provided by the invention can also carry out filling nitrogen process before embedding.
The present invention innovates part and is: the present invention is taking Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside and general flavone content as index; former stone sulphur method has been improved; not only reach the object removing the impurity such as tannin, and the flavones ingredient remained greatly in injection liquid. Herba Hedyotidis Diffusae injection general flavone content height provided by the invention, steady quality, anti-inflammation test result shows that effect is better than former preparation.
By example by experiment, the invention will be further described below.
Experimental example 1 stone sulphur method is on the impact of flavones ingredient content in extracting solution
1, sample preparation
Sample 1: get Spreading Hedyotis Herb 1000g, uses 80% extraction using alcohol, and extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, refrigerates 12 hours, filters, and filtrate is adjusted to neutrality with 50% sulphuric acid soln, adds water to 1000ml, filters, to obtain final product;
Sample 2: get Spreading Hedyotis Herb 1000g, uses 80% extraction using alcohol, and extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 7, refrigerating 12 hours, filter, filtrate is adjusted to neutrality with 50% sulphuric acid soln, add water to 1000ml, filter, to obtain final product;
Sample 3: get Spreading Hedyotis Herb 1000g, uses 80% extraction using alcohol, and extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 8, refrigerating 12 hours, filter, filtrate is adjusted to neutrality with 50% sulphuric acid soln, add water to 1000ml, filter, to obtain final product;
Sample 4: get Spreading Hedyotis Herb 1000g, uses 80% extraction using alcohol, and extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 9, refrigerating 12 hours, filter, filtrate is adjusted to neutrality with 50% sulphuric acid soln, add water to 1000ml, filter, to obtain final product;
Sample 5: get Spreading Hedyotis Herb 1000g, uses 80% extraction using alcohol, and extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 10, refrigerating 12 hours, filter, filtrate is adjusted to neutrality with 50% sulphuric acid soln, add water to 1000ml, filter, to obtain final product.
2, flavones ingredient detection
Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside (chromocor compound 1) content adopts HPLC method to measure, and chromatographic condition is: take octadecylsilane chemically bonded silica as weighting agent; Taking acetonitrile-0.3% glacial acetic acid aqueous solution (18:82) as moving phase; Determined wavelength is 330nm.
Total flavones measuring method is: precision measures sample 5ml, it is added on processed good polyamide column (50 orders, 2g, internal diameter 12��15mm, wet method dress post) on, use 50ml water elution, abandon elutriant, use 70% ethanol elution, collect elutriant and it is about 25ml, put in 25ml measuring bottle, the alcohol dilution adding 70% is to scale, shake even, precision measures 5ml respectively, put first, in second two 25ml measuring bottles, the sodium nitrite solution 1ml that adds 5% in first bottle, shake even, place 6 minutes, the aluminum nitrate solution 1ml that adds 10%, shake even, place 6 minutes, in first, each hydro-oxidation sodium test solution 10ml in second two bottles, add alcohol dilution again to scale, shake even, place 15 minutes, according to spectrophotometry (version " Chinese Pharmacopoeia " annex V B in 2010), taking second bottle as blank, optical density is measured at the wavelength place of 507nm.
Measurement result is in table 1:
Table 1 flavones ingredient measurement result
| Title | Chromocor compound 1 (�� g/ml) | Total flavones A507 |
| Sample 1 | 7.8 | 0.316 |
| Sample 2 | 55.3 | 0.605 |
| Sample 3 | 55.4 | 0.613 |
| Sample 4 | 43.8 | 0.539 |
| Sample 5 | 27.2 | 0.424 |
As shown in Table 1, when Spreading Hedyotis Herb extracting solution is first by milk of lime adjust ph to 12, then by 50% sulphuric acid soln adjust ph to 7-8, refrigeration, filters the flavones ingredient content height in the filtrate obtained.
Experimental example 2 alcohol precipitation process is studied
1, sample preparation
Get Spreading Hedyotis Herb 1200g, use 80% extraction using alcohol, extracting solution concentrates to 300ml, by milk of lime adjust ph to 12, then by 50% sulphuric acid soln adjust ph to 8, refrigerate 12 hours, filtering, filtrate, by 50% sulphuric acid soln adjust ph to 3, leaves standstill 12 hours, filter, filtrate to 6.0-6.5, is divided into three parts by 40% sodium hydroxide solution adjust ph, and adding ethanol to alcohol content respectively is 75%, 80%, 85%, refrigerate 24 hours, filtering, filtrate recycling ethanol, is diluted with water to 400ml, filter, to obtain final product.
2, total flavones and total solids test
Total flavones measuring method is: precision measures sample 10ml, it is added on processed good polyamide column (50 orders, 2g, internal diameter 12��15mm, wet method dress post) on, use 50ml water elution, abandon elutriant, use 70% ethanol elution, collect elutriant and it is about 25ml, put in 25ml measuring bottle, the alcohol dilution adding 70% is to scale, shake even, precision measures 5ml respectively, put first, in second two 25ml measuring bottles, the sodium nitrite solution 1ml that adds 5% in first bottle, shake even, place 6 minutes, the aluminum nitrate solution 1ml that adds 10%, shake even, place 6 minutes, in first, each hydro-oxidation sodium test solution 10ml in second two bottles, add alcohol dilution again to scale, shake even, place 15 minutes, according to spectrophotometry (version " Chinese Pharmacopoeia " annex V B in 2010), taking second bottle as blank, optical density is measured at the wavelength place of 507nm.
Total solids test method is: precision measures this product 10ml, puts in the furnace pot of constant weight, steams dry in water-bath, 105 DEG C of dryings 3 hours, moves and cools 30 minutes to moisture eliminator, rapid weighed weight, calculates, to obtain final product.
Measurement result is in table 2:
Table 2 total flavones and total solids test result
| Title | Total flavones A507nm | Total solids (mg/ml) |
| 75% alcohol precipitation sample | 0.857 | 39.8 |
| 80% alcohol precipitation sample | 0.833 | 34.3 |
| 85% alcohol precipitation sample | 0.745 | 30.7 |
As shown in Table 2,75% alcohol precipitation is close with 80% alcohol precipitation sample general flavone content, but 75% alcohol precipitation sample total solid amount is big, therefore alcohol precipitation concentration preferably 80%.
Experimental example 3 adds oxidation inhibitor and fills nitrogen to the impact of liquid PH value
Get the liquid refined and it is divided into 6 parts, 2 parts one group, the first group of oxidation inhibitor that adds 0.1%, the 2nd group of oxidation inhibitor that adds 0.2%, the 3rd group of oxidation inhibitor that adds 0.2% and fill nitrogen, in each group, before 2 parts of sample sterilizings, PH value is adjusted to 6.9 and 7.2,115 DEG C of sterilizings 30 minutes respectively, measure PH value after 6 parts of sample sterilizings, the results are shown in Table 3.
PH pH-value determination pH result after table 36 part sample sterilizing
As shown in Table 3, liquid adds oxidation inhibitor and fills nitrogen, and the change of sterilization process liquid PH value is minimum.
Experimental example 4 anti-inflammatory action is studied
1, p-Xylol causes the impact of mice ear
Get Kunming kind female mice 30, body weight 18��22g, it is divided into 3 groups at random, often organize 10. Respectively abdominal injection embodiment 1 Herba Hedyotidis Diffusae injection, comparative example 1 Herba Hedyotidis Diffusae injection group-and etc. the physiological saline of volume, after 20min, proinflammatory agent dimethylbenzene 0.04ml is evenly applied to the left ear two sides of mouse, right ear is used in contrast. Put to death mouse after causing scorching 30min, get left and right auricle with diameter 8mm punch tool and weigh, taking the difference of two auricle weight as inflammatory swelling degree index, compare group difference, the results are shown in Table 4.
Table 4 Herba Hedyotidis Diffusae injection p-Xylol causes the impact (X �� S) of mice ear
| Group | Number of animals (n) | Dosage (g crude drug kg-1) | Swelling (mg) |
| Physiological saline group | 10 | ---- | 22.90��4.09 |
| Embodiment 1 Herba Hedyotidis Diffusae injection group | 10 | 0.4 | 7.13��3.23** |
| Comparative example 1 Herba Hedyotidis Diffusae injection group | 10 | 0.4 | 13.81��2.52* |
Note: compare * * P < 0.01, * P < 0.05 with physiological saline group
As shown in Table 4, comparing with physiological saline group, embodiment 1 Herba Hedyotidis Diffusae injection p-Xylol causes mice ear very significantly restraining effect (P < 0.01), and effect is better than comparative example 1 Herba Hedyotidis Diffusae injection.
2, on the impact of rat paw edema caused by egg white
Body weight 130��160g rat 24, male and female are all used, it is divided into 3 groups at random, respectively abdominal injection embodiment 1 Herba Hedyotidis Diffusae injection, comparative example 1 Herba Hedyotidis Diffusae injection group-and etc. the physiological saline of volume, all inflammation is caused in the right sufficient plantar subcutaneous injection 20% fresh albumen 0.1ml of rat after 30min, respectively before causing inflammation and cause scorching after 0.5, l, 2,3,4,5h rat foot claw instrument measure right back sufficient pawl volume, so that before and after scorching, volume differences is as swelling (inflammation index), the results are shown in Table 5.
Table 5 Herba Hedyotidis Diffusae injection is on the impact of rat paw edema caused by egg white
Note: compare with physiological saline group, * P < 0.05, * * P < 0.01.
As shown in Table 5, comparing with physiological saline group, the foot pawl swelling of fresh albumen induced rat is had obvious restraining effect by embodiment 1 Herba Hedyotidis Diffusae injection, and effect is better than comparative example 1 Herba Hedyotidis Diffusae injection.
Embodiment
Following embodiment is for illustration of the present invention, but is not used for limiting the scope of the invention.
Embodiment 1 Herba Hedyotidis Diffusae injection
Get Spreading Hedyotis Herb 1000g, pulverize into meal, according to the percolation (version " Chinese Pharmacopoeia " annex I O in 2010) under fluid extract and extractum item, use 80% ethanol as solvent, flood 24 hours, slowly ooze and filter, percolate concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 8, refrigerate 12 hours, filter, filtrate is by 50% sulphuric acid soln adjust ph to 3, leave standstill 12 hours, filter, filtrate by 40% sodium hydroxide solution adjust ph to 6.0-6.5, adding ethanol makes alcohol content reach 80%, refrigerate 24 hours, filter, filtrate recycling ethanol also concentrates to 250ml, add water to 500ml, add 1.0g gac, stir even, filter, filtrate is with 40% sodium hydroxide solution adjust ph to 6.5��7.0, add 10g Polysorbate 80 and 1g sodium bisulfite, fully stir even, inject water to 1000ml, filter, embedding, 115 DEG C of sterilizings, obtain.
Detected result: every ml soln is containing 10-deacetyl asperulosidic acid methyl ester 43 �� g, containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside 45 �� g.
Wherein, 10-deacetyl asperulosidic acid methyl ester adopts HPLC method to measure, and chromatographic condition is: take octadecylsilane chemically bonded silica as weighting agent; Taking acetonitrile-water (3:97) as moving phase; Determined wavelength is 236nm.
Embodiment 2 Herba Hedyotidis Diffusae injection
Get Spreading Hedyotis Herb 1000g, with 60% alcohol reflux 2 times, extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 7, refrigerate 12 hours, filter, filtrate is by 50% sulphuric acid soln adjust ph to 3, leave standstill 12 hours, filter, filtrate by 40% sodium hydroxide solution adjust ph to 6.0-6.5, adding ethanol makes alcohol content reach 85%, refrigerate 24 hours, filter, filtrate recycling ethanol also concentrates to 250ml, add water to 500ml, add 1.5g gac, stir even, filter, filtrate is with 40% sodium hydroxide solution adjust ph to 6.5��7.0, add 12g Polysorbate 80 and 1.5g sodium bisulfite, fully stir even, inject water to 1000ml, filter, fill nitrogen, embedding, 115 DEG C of sterilizings, obtain.
Detected result: every ml soln is containing 10-deacetyl asperulosidic acid methyl ester 35 �� g, containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside 38 �� g.
Embodiment 3 Herba Hedyotidis Diffusae injection
Get Spreading Hedyotis Herb 1000g, with 80% alcohol reflux 2 times, extracting solution concentrates to 250ml, by milk of lime adjust ph to 12, again by 50% sulphuric acid soln adjust ph to 10, refrigerate 12 hours, filter, filtrate is by 50% sulphuric acid soln adjust ph to 3, leave standstill 12 hours, filter, filtrate by 40% sodium hydroxide solution adjust ph to 6.0-6.5, adding ethanol makes alcohol content reach 75%, refrigerate 24 hours, filter, filtrate recycling ethanol also concentrates to 250ml, add water to 500ml, add 0.5g gac, stir even, filter, filtrate is with 40% sodium hydroxide solution adjust ph to 6.5��7.0, add 8g Polysorbate 80 and 0.5g sodium bisulfite, fully stir even, inject water to 1000ml, filter, fill nitrogen, embedding, 115 DEG C of sterilizings, obtain.
Detected result: every ml soln is containing 10-deacetyl asperulosidic acid methyl ester 45 �� g, containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside 32 �� g.
Comparative example 1 Herba Hedyotidis Diffusae injection
Get Spreading Hedyotis Herb 1000g, pulverize into meal, according to the percolation (version " Chinese Pharmacopoeia " annex I O in 2010) under fluid extract and extractum item, use 80% ethanol as solvent, flood 24 hours, slowly ooze and filter, liquid of filtering concentrates to 250ml, by milk of lime adjust ph to 12, refrigerate 12 hours, filter, filtrate is 3 by 50% sulphuric acid soln adjust ph, leave standstill 12 hours, filter, filtrate is adjusted to neutrality with 40% sodium hydroxide solution again, add ethanol 2000ml, refrigerate 24 hours, filter, filtrate concentrates to 250ml, add water to 500ml, add 1.0g gac, stir even, filter, filtrate is 6.5��7.0 by 40% sodium hydroxide solution adjust ph, add 10g Polysorbate 80, 1g sodium bisulfite, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, obtain.
Detected result: every ml soln is containing 10-deacetyl asperulosidic acid methyl ester 42 �� g, containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside 7 �� g.
Claims (6)
1. a Herba Hedyotidis Diffusae injection, it is the sterile water solution being made up through extracting of Spreading Hedyotis Herb, it is characterised in that: every ml soln is no less than 30 �� g containing 10-deacetyl asperulosidic acid methyl ester; Every ml soln is no less than 30 �� g containing Quercetin-3-O-[2-O-(6-O-E-mustard acyl)-��-D-glucopyranosyl]-��-D-glucopyranoside, and preparation method is as follows:
(1) get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, obtain extracting solution;
(2) extracting solution is through concentrated, obtains concentrated solution I;
(3) concentrated solution I is first by milk of lime adjust ph to 12, then by sulfur acid aqueous solution adjust ph to 7-10, refrigeration, filters, obtain filtrate I;
(4) filtrate I is by sulfur acid aqueous solution adjust ph to 2-4, leaves standstill, and filters, obtains filtrate II;
(5) filtrate II adjust ph is to 5-7, adds ethanol and makes alcohol content reach 65%��90%, refrigeration, filters, and concentrating filter liquor, obtains concentrated solution II;
(6) concentrated solution II adds water to the 1-4 times amount of original volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, to obtain final product.
2. prepare the method for Herba Hedyotidis Diffusae injection as claimed in claim 1, it is characterised in that comprise the following steps:
(1) get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, obtain extracting solution;
(2) extracting solution is through concentrated, obtains concentrated solution I;
(3) concentrated solution I is first by milk of lime adjust ph to 12, then by sulfur acid aqueous solution adjust ph to 7-10, refrigeration, filters, obtain filtrate I;
(4) filtrate I is by sulfur acid aqueous solution adjust ph to 2-4, leaves standstill, and filters, obtains filtrate II;
(5) filtrate II adjust ph is to 5-7, adds ethanol and makes alcohol content reach 65%��90%, refrigeration, filters, and concentrating filter liquor, obtains concentrated solution II;
(6) concentrated solution II adds water to the 1-4 times amount of original volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, to obtain final product.
3. preparation method as claimed in claim 2, it is characterised in that comprise the following steps:
(1) get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, obtain extracting solution;
(2) extracting solution is through concentrated, obtains concentrated solution I;
(3) concentrated solution I is first by milk of lime adjust ph to 12, then by sulfur acid aqueous solution adjust ph to 7-8, refrigeration, filters, obtain filtrate I;
(4) filtrate I is by sulfur acid aqueous solution adjust ph to 2-4, leaves standstill, and filters, obtains filtrate II;
(5) filtrate II adjust ph is to 5-7, adds ethanol and makes alcohol content reach 65%��90%, refrigeration, filters, and concentrating filter liquor, obtains concentrated solution II;
(6) concentrated solution II adds water to the 1-4 times amount of original volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, to obtain final product.
4. preparation method as claimed in claim 2, it is characterised in that comprise the following steps:
(1) get Spreading Hedyotis Herb 1000g, extract with 10%-95% aqueous ethanolic solution, obtain extracting solution;
(2) extracting solution is through concentrated, obtains concentrated solution I;
(3) concentrated solution I is first by milk of lime adjust ph to 12, then by sulfur acid aqueous solution adjust ph to 7-8, refrigeration, filters, obtain filtrate I;
(4) filtrate I is by sulfur acid aqueous solution adjust ph to 2-4, leaves standstill, and filters, obtains filtrate II;
(5) filtrate II adjust ph is to 5-7, adds ethanol and makes alcohol content reach 75%��85%, refrigeration, filters, and concentrating filter liquor, obtains concentrated solution II;
(6) concentrated solution II adds water to the 1-4 times amount of original volume, add the gac of 0.1%��0.4%, stir even, filter, filtrate adjust ph to 6.5��7.5, add the solubilizing agent of 0.1%��2.0% and the oxidation inhibitor of 0.05%-0.2%, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, to obtain final product.
5. preparation method as claimed in claim 2, it is characterised in that comprise the following steps:
(1) get Spreading Hedyotis Herb 1000g, use 80% extraction using alcohol, obtain extracting solution;
(2) extracting solution concentrates to 250ml, obtains concentrated solution I;
(3) concentrated solution I is first by milk of lime adjust ph to 12, then by 50% sulphuric acid soln adjust ph to 8, refrigerates 12-24 hour, filters, obtains filtrate I;
(4) filtrate I is by 50% sulphuric acid soln adjust ph to 3, leaves standstill 12-24 hour, filters, obtains filtrate II;
(5) filtrate II is by 40% sodium hydroxide solution adjust ph to 6.0-6.5, adds ethanol and makes alcohol content reach 80%, refrigerates 24-72 hour, filters, and filtrate concentrates to 250ml, obtains concentrated solution II;
(6) concentrated solution II adds water to 500ml, add 0.5g-1.5g gac, stir even, filter, filtrate is with 40% sodium hydroxide solution adjust ph to 6.5��7.0, add 10g Polysorbate 80 and 1g sodium bisulfite, fully stir even, inject water to 1000ml, filter, embedding, sterilizing, to obtain final product.
6. the preparation method as described in as arbitrary in claim 2-5, it is characterised in that: carry out before embedding filling nitrogen process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410174335.5A CN103948717B (en) | 2014-04-29 | 2014-04-29 | A kind of Herba Hedyotidis Diffusae injection and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410174335.5A CN103948717B (en) | 2014-04-29 | 2014-04-29 | A kind of Herba Hedyotidis Diffusae injection and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103948717A CN103948717A (en) | 2014-07-30 |
| CN103948717B true CN103948717B (en) | 2016-06-01 |
Family
ID=51326158
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410174335.5A Active CN103948717B (en) | 2014-04-29 | 2014-04-29 | A kind of Herba Hedyotidis Diffusae injection and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103948717B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336983A (en) * | 2007-07-02 | 2009-01-07 | 广西壮族自治区花红药业股份有限公司 | Oldenlandia and quality control method of preparation containing oldenlandia |
| CN102078411A (en) * | 2009-11-30 | 2011-06-01 | 北京振国天仙生物技术有限公司 | Preparation method of spreading hedyotis herb injection |
-
2014
- 2014-04-29 CN CN201410174335.5A patent/CN103948717B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336983A (en) * | 2007-07-02 | 2009-01-07 | 广西壮族自治区花红药业股份有限公司 | Oldenlandia and quality control method of preparation containing oldenlandia |
| CN102078411A (en) * | 2009-11-30 | 2011-06-01 | 北京振国天仙生物技术有限公司 | Preparation method of spreading hedyotis herb injection |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103948717A (en) | 2014-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112716989B (en) | Celery seed extract and preparation method and application thereof | |
| US9186385B2 (en) | Plant extract compositions for prevention and treatment of influenza | |
| Alajmi et al. | Comparative anticancer and antimicrobial activity of aerial parts of Acacia salicina, Acacia laeta, Acacia hamulosa and Acacia tortilis grown in Saudi Arabia | |
| CN102552644A (en) | Anti-tumor use, preparation method and composition of garlic total polysaccharide | |
| CN1116293C (en) | Preparation and application of dihydromyricetrin | |
| CN101099566B (en) | Lactucin and its preparation method and application | |
| CN101019893A (en) | Process of enriching effective antitumor part of periplaneta americana with polyamide | |
| CN101890084B (en) | Semen nigellae total glycoside extract and preparation method and application thereof | |
| CN102258598B (en) | Medicine prepared by active part of pawpaw, its preparation method and its application | |
| CN101972385B (en) | Method for preparing general flavone in star-of-Bethlehem and application thereof to antitumor, anti-inflammatory and analgesic medicines | |
| CN107090049B (en) | Arborvitae total starches and its preparing the purposes in immunosuppressive drug | |
| CN100443498C (en) | Use of anti-inflammatory medicine for scheelite total saponin and its saponin compound | |
| CN111635442B (en) | Method for preparing three monomer compounds from medicinal plant pachyrhizus and in-vitro antioxidant effect thereof | |
| CN101347424A (en) | Use of luteolin in preparing anticomplement medicament | |
| CN100574792C (en) | A kind of effective ingredient detection method of Chinese medicine composition | |
| CN102671059A (en) | Smilax extract, and preparation method and application thereof | |
| CN103948717B (en) | A kind of Herba Hedyotidis Diffusae injection and its preparation method | |
| CN101278970B (en) | Method for preparing Elsholtzia bodinieri flavonoid and applications | |
| CN104069194B (en) | A kind of Chinese medicine composition with antitumaous effect and its production and use | |
| CN103091412B (en) | Method for detecting ginkgolide effective parts | |
| CN103830374A (en) | Application of three-leaf glycolipid-removal medicine in hyperuricemia | |
| CN103120721B (en) | Chinese medicinal composition for treating wind-heat common cold and preparation method and application thereof | |
| CN106580935A (en) | Uses of aryl-substituted phenylpropanoid-based compounds in preparation of anti-complement drugs | |
| CN102125614A (en) | Preparation method of traditional Chinese medicine composition for treating common cold of children | |
| CN105168509A (en) | Preparation technology of high-content compound herba houttuyniae mixture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 335200 north of national highway 320, Jiaotong North Road, Yujiang District, Yingtan City, Jiangxi Province Patentee after: Jiangxi Kangenbei tianshikang Pharmaceutical Co.,Ltd. Address before: 335000 No.11, wanbaozhi Road, Yingtan City, Jiangxi Province Patentee before: Jiangxi Herbi-Sky Co.,Ltd. |
|
| CP03 | Change of name, title or address |