CN111419887A - Selaginella chinensis total biflavone solid dispersion and preparation method thereof - Google Patents
Selaginella chinensis total biflavone solid dispersion and preparation method thereof Download PDFInfo
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- CN111419887A CN111419887A CN202010153763.5A CN202010153763A CN111419887A CN 111419887 A CN111419887 A CN 111419887A CN 202010153763 A CN202010153763 A CN 202010153763A CN 111419887 A CN111419887 A CN 111419887A
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Abstract
The invention discloses a selaginella doederleinii hieron total biflavone solid dispersion and a preparation method thereof, belongs to the technical field of medicines, and relates to a selaginella doederleinii hieron total biflavone solid dispersion and a preparation method thereof. The invention adopts a solvent method, firstly adding the selaginella doederleinii hieron total biflavone extract powder into ethanol for dissolving, then dripping the selaginella doederleinii hieron total biflavone extract powder into a carrier PVP-K30 solution, and preparing a solid dispersion by a solvent volatilization method; and preparing the solid dispersion capsule by adopting a direct filling method. The ratio of selaginella doederleinii general biflavone to PVP-K30 is 1: 3-1: 10. compared with the bulk drugs, the prepared solid dispersion preparation has obviously increased in-vitro dissolution rate and improved oral bioavailability; solves the problems of low dissolution rate and low utilization rate of the selaginella doederleinii hieron total biflavone drug.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a selaginella doederleinii hieron total biflavone solid dispersion and a preparation method thereof.
Background
Herba Selaginellae Doederleinii Hieron is a whole herb of Selaginella tamariscina (Thunb.) Vahl of Selaginellaceae, also called Selaginella tamariscina, herba Gelidonii, cacumen Myricariae Germanicae, and ramulus et folium Platycladi, and has effects of clearing away heat and toxic materials, dispelling pathogenic wind, removing dampness, resisting cancer, and stopping bleeding. The medicine is mainly used for treating various cancers such as nasopharyngeal carcinoma, lung cancer, skin cancer, gastric cancer and the like. The selaginella doederleinii hieron contains various active substances, the selaginella doederleinii hieron total biflavone active component extract is prepared through earlier researches, and further researches show that the selaginella doederleinii hieron total biflavone active component extract has remarkable anti-tumor activity in vitro and in vivo, shows the characteristics of high efficiency and low toxicity, and is worthy of further research and development. However, previous researches find that the solubility of the selaginella doederleinii general biflavone extract in water is low, the in vivo dissolution rate is low, and the bioavailability is poor. In order to improve the dissolution rate of the selaginella doederleinii hieron total biflavone and improve the bioavailability of the selaginella doederleinii hieron total biflavone, the problem of low solubility in water must be solved firstly. The solid dispersion technology is an effective means for improving solubility and bioavailability, and the total biflavone in the selaginella doederleinii hieron is prepared into the solid dispersion, so that the solubility and the dissolution rate of the selaginella doederleinii hieron can be improved, and the absorption and the bioavailability of a medicine by an organism can be improved.
Disclosure of Invention
The invention aims to provide a selaginella general biflavone solid dispersion and a preparation method thereof aiming at the problems that the solubility of a selaginella general biflavone extract in water is low, the dissolution rate in vivo is low, and the bioavailability is poor.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing herba Selaginellae Doederleinii total biflavone solid dispersion comprises the following steps:
(1) weighing the components in a mass ratio of 1: 3-1: 10 of selaginella doederleinii general biflavone extract and PVP-K30;
(2) dissolving with appropriate amount of 80-100 wt% ethanol solution, and slowly dripping the obtained herba Selaginellae Doederleinii total biflavone extract solution into PVP-K30 solution as carrier;
(3) ultrasonic treating for 10-20 min for mixing, rotary steaming at 60 deg.C, and removing ethanol;
(4) vacuum drying at 45-55 deg.C, pulverizing, and sieving with 80 mesh sieve to obtain herba Selaginellae Doederleinii total biflavone solid dispersion.
The mass ratio of the selaginella general biflavone extract to the PVP-K30 in the step (1) is preferably 1: 5.
the ethanol in the step (2) is preferably absolute ethanol.
The ultrasonic treatment time in the step (3) is preferably 20 min.
The vacuum drying temperature in the step (4) is preferably 50 ℃.
The preparation method of the invention prepares the selaginella doederleinii hieron total biflavone solid dispersion.
Specifically, the invention adopts the following technical scheme:
weighing the components in a mass ratio of 1: dissolving the selaginella doederleinii hieron total biflavone extract and PVP-K30 with a proper amount of 80-100% ethanol solution respectively, slowly dripping the total biflavone extract solution into a carrier PVP-K30 solution, performing ultrasonic treatment for 10-20 min to fully mix the two solutions, performing rotary evaporation at a constant temperature of 60 ℃, removing ethanol, performing vacuum drying at a temperature of 45-55 ℃, crushing, sieving with an 80-mesh sieve to prepare a semi-finished product, and placing the semi-finished product in a dryer for later use.
Directly filling the semi-finished product powder into hollow capsules to obtain the selaginella doederleinii hieron total biflavone capsules.
The invention has the beneficial effects that: the preparation method prepares the selaginella doederleinii hieron total biflavone extract into the solid dispersion, is pioneering in the aspect of selaginella doederleinii hieron extract preparation, greatly improves the solubility and dissolution rate of the prepared solid dispersion preparation compared with the raw material of the extract, effectively improves the absorption and bioavailability of the selaginella doederleinii hieron total biflavone extract in an organism, and is suitable for being used as an oral preparation for treating cancers.
Drawings
FIG. 1 is a graph showing the dissolution profiles of the total flavonoids (extract) of Selaginella chinensis (Thunb.) DC, the Physical Mixture (PM) of the total flavonoids (extract) of Selaginella chinensis (Thunb.) DC with PVP-K30, and the Solid Dispersion (SD) of the total flavonoids (extract) of Selaginella chinensis (Thunb.) DC according to the present invention.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
A method for preparing herba Selaginellae Doederleinii total biflavone solid dispersion comprises the following steps:
pulverizing dried herba Selaginellae Doederleinii whole herb, sieving with No. 3 sieve, extracting with 45 times of 70 wt% ethanol (45 ml70 wt% ethanol for 1g powder) at 85 deg.C for 2 times, each for 1.5 hr. Concentrating the extracting solution to obtain clear paste with the relative density of 1.10-1.15 (60 ℃); sequentially extracting with petroleum ether and ethyl acetate of equal volume for 3 times, respectively, collecting ethyl acetate layer solution, rotary evaporating at 60 deg.C to dryness, making into extract, freeze drying, and pulverizing. (the general Doripyriferone extract of Selaginella pulvinata used in the following examples was prepared in the same manner)
Weighing the components in a mass ratio of 1: dissolving herba Selaginellae Doederleinii total biflavone extract and polyvidone (PVP-K30) with appropriate amount of anhydrous ethanol, slowly dripping herba Selaginellae Doederleinii total biflavone extract solution into PVP-K30 solution as carrier, ultrasonic treating for 20min for mixing, rotary steaming at 60 deg.C, removing ethanol, vacuum drying at 50 deg.C under reduced pressure, pulverizing, and sieving with 80 mesh sieve.
Example 2
A method for preparing herba Selaginellae Doederleinii total biflavone solid dispersion comprises the following steps:
weighing the components in a mass ratio of 1:3 dissolving the total flavonoids of selaginella doederleinii hieron and PVP-K30 in 90wt% ethanol solution, slowly dripping the total flavonoids of selaginella doederleinii hieron solution into the PVP-K30 solution as carrier, ultrasonic treating for 15min for mixing, rotary steaming at 60 deg.C, removing ethanol, vacuum drying at 55 deg.C under reduced pressure, pulverizing, and sieving with 80 mesh sieve.
Example 3
Weighing the components in a mass ratio of 1: 4 dissolving herba Selaginellae Doederleinii total biflavone extract and PVP-K30 with appropriate amount of 80wt% ethanol solution, slowly dripping herba Selaginellae Doederleinii total biflavone extract solution into PVP-K30 solution as carrier, ultrasonic treating for 10 min for thoroughly mixing, rotary steaming at 60 deg.C, removing ethanol, vacuum drying at 55 deg.C under reduced pressure, pulverizing, and sieving with 80 mesh sieve.
Example 4
And (3) taking 500g of the sieved selaginella doederleinii hieron total biflavone solid dispersion prepared in the embodiment 3, and encapsulating the 500g of selaginella doederleinii hieron total biflavone solid dispersion to prepare 1000 capsules.
Example 5
Dissolution test of solid dispersion, total biflavone extract and physical mixture
Taking a proper amount of the selaginella doederleinii hieron total biflavone solid dispersion prepared in the example 1, the selaginella doederleinii hieron total biflavone extract and a physical mixture of the selaginella doederleinii hieron total biflavone extract and PVP-K30, taking a phosphate buffer solution with the pH value of 900 m L and the pH value of 6.8 as a dissolution medium, performing a slurry method at the rotating speed of 75 r/min at the temperature of 37 +/-0.5 ℃, sampling 5m L at the time of 5min, 10 min, 20min, 30 min, 45 min, 60 min, 90 min and 120 min respectively, supplementing a homothermal medium of 5m L, filtering with a 0.45 mu m microporous filter membrane, taking the corresponding dissolution medium as a blank control, measuring the absorbance at 340 nm by an ultraviolet spectrophotometry, calculating the cumulative dissolution rate of the total biflavone.
The results in fig. 1 show that the Solid Dispersion (SD), the Physical Mixture (PM), and the selaginella doederleinii general biflavone extract have a large dissolution difference in a phosphate buffer solution with a pH of 6.8, the extract is basically insoluble, the dissolution of the physical mixture is greatly improved compared with the extract, but is obviously lower than the dissolution of the solid dispersion, which indicates that the selaginella doederleinii general biflavone extract and PVP-K30 in the solid dispersion form a relatively stable effect, and thus the dissolution performance is greatly improved.
Claims (6)
1. A method for preparing selaginella doederleinii hieron total biflavone solid dispersion comprises the following steps:
(1) weighing the components in a mass ratio of 1: 3-1: 10 of selaginella doederleinii general biflavone extract and PVP-K30; (2) dissolving with appropriate amount of 80-100 wt% ethanol solution, and slowly dripping the obtained herba Selaginellae Doederleinii total biflavone extract solution into PVP-K30 solution as carrier; (3) ultrasonic treating for 10-20 min for mixing, rotary steaming at 60 deg.C, and removing ethanol; (4) vacuum drying at 45-55 deg.C, pulverizing, and sieving with 80 mesh sieve.
2. The method according to claim 1, wherein the mass ratio of the selaginella doederleinii hieron total biflavone extract to the PVP-K30 in the step (1) is 1: 3-1: 10, preferably in a ratio of 1: 5.
3. the method according to claim 1, wherein the concentration of the ethanol solution in the step (2) is 80wt% to 100 wt%; the preferred ethanol solution is absolute ethanol.
4. The production method according to claim 1, characterized in that the sonication time in step (3) is 10-20 min; the preferred sonication time is 20 min.
5. The method according to claim 1, wherein the vacuum decompression drying temperature in the step (4) is 45 to 55 ℃; the preferred temperature for vacuum drying is 50 ℃.
6. The method according to any one of claims 1-5, wherein the selaginella doederleinii hieron total biflavone solid dispersion is obtained.
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| CN202010153763.5A CN111419887A (en) | 2020-03-07 | 2020-03-07 | Selaginella chinensis total biflavone solid dispersion and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1726945A (en) * | 2004-08-03 | 2006-02-01 | 深圳海王药业有限公司 | Solid dispersion of extractive of general flavone of Balsamiferou Blumea Herb |
| CN110478379A (en) * | 2019-06-21 | 2019-11-22 | 福建医科大学 | A kind of total biflavone proliposome of selaginella doederlleini and preparation method thereof |
-
2020
- 2020-03-07 CN CN202010153763.5A patent/CN111419887A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1726945A (en) * | 2004-08-03 | 2006-02-01 | 深圳海王药业有限公司 | Solid dispersion of extractive of general flavone of Balsamiferou Blumea Herb |
| CN110478379A (en) * | 2019-06-21 | 2019-11-22 | 福建医科大学 | A kind of total biflavone proliposome of selaginella doederlleini and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| BING CHEN等: "Improved solubility, dissolution rate, and oral bioavailability of main biflavonoids from Selaginella doederleinii extract by amorphous solid dispersion", 《DRUG DELIVERY》 * |
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