CN113244278B - Preparation method of nanoscale quassia powder - Google Patents
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Abstract
The invention discloses a preparation method of nano-scale quassia powder, belonging to the technical field of traditional Chinese medicines. The method comprises the following steps: s01, cleaning the quassia, drying and crushing; s02, pretreating with acetone and absolute ethyl alcohol, and drying; s03, preparing quassia water suspension; s04, cooling; s05, processing by an ultrasonic pulverizer; s06, filtering, and crushing the filtrate by using a nano collider; s07, drying to obtain nanometer Chinese medicinal powder. The preparation method of the nano-scale traditional Chinese medicine powder provided by the invention obtains the nano-scale powder of the traditional Chinese medicine quassia. The preparation method of the nano-scale traditional Chinese medicine powder disclosed by the invention finds the unexpected technical effect of the steps of pretreatment and low-temperature control of acetone and absolute ethyl alcohol.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a preparation method of nano-scale quassia powder.
Background
The quassia injection has the effects of clearing heat, detoxifying and diminishing inflammation. Can be used for treating common cold, upper respiratory infection, acute tonsillitis, enteritis, and bacillary dysentery. The main raw material is quassia. Ramulus Et folium Picrasmae is the dried branch and leaf of ramulus Et folium Picrasmae of Simaroubaceae. Collected in summer and autumn and dried.
In the preparation process of the quassia injection, the particle size of quassia powder can greatly influence picfeltrarin IAThe extraction also influences the subsequent separation process, and the nano-scale quassia powder is required to be obtained quickly, efficiently and energy-efficiently.
CN1672720A discloses a method for preparing a Chinese medicinal nanometer preparation. Wherein, the suspension is crushed by ultrasonic waves, so that the particles of the medicinal materials in the suspension are smaller than 10 μm, and the suspension is filtered to obtain filtrate; then crushing by a nanometer collider to ensure that the particle size of the medicinal materials reaches the nanometer level, thus obtaining the nanometer traditional Chinese medicine suspension. The patent obtains the nanometer powder of medicinal materials such as astragalus, pearl, ginseng, cortex acanthopanacis and the like.
Disclosure of Invention
When the researchers of the invention apply the nano collider crushing technology to the traditional Chinese medicine quassia, the researchers find that nano-scale powder is difficult to obtain by adopting the method.
The invention discloses a preparation method of nano-scale traditional Chinese medicine powder, which is characterized by comprising the following steps:
s01, cleaning the quassia, drying and crushing;
s02, pretreating with acetone and absolute ethyl alcohol, and drying;
s03, preparing quassia water suspension;
s04, cooling;
s05, processing by an ultrasonic pulverizer;
s06, filtering, and crushing the filtrate by using a nano collider;
s07, drying to obtain nanometer Chinese medicinal powder.
In some preferred embodiments of the present invention, in S01, the mixture is initially chopped to a particle size of 450-550 μm.
In some preferred embodiments of the present invention, S02 is prepared by soaking in acetone, drying, soaking in absolute ethanol, and drying.
In some preferred embodiments of the invention, 4-6 times of acetone by weight is added into S02, soaked for 12-16h and dried; adding 4-6 times of anhydrous alcohol, soaking for 4-6 hr, and drying.
In some preferred embodiments of the invention, in S03, the weight ratio of quassia to water in the aqueous suspension of quassia is 1: (40-55).
In some preferred embodiments of the invention, in S04, the quassia suspension is temperature-controlled to below 2 ℃
In some preferred embodiments of the present invention, in S05, the ultrasonic pulverizer is processed to pulverize the quassia particles into a suspension of less than 10 μm; the temperature was controlled to below 2 ℃ with an ice bath throughout.
In some preferred embodiments of the present invention, in S05, filtering is performed with a 300-mesh sieve, the filtrate is collected, pulverized with a nano collider, and treated at a pressure of 130Mpa and a working speed of 300rpm for 2 hours.
In some preferred embodiments of the present invention, 0.05-0.2% (w/v) lecithin, more preferably 0.08-0.15% (w/v) lecithin, is added to the filtrate in S06.
In some preferred embodiments of the present invention, in S02, the time T2 of the absolute ethanol soak is determined by the following formula:
wherein T1 is the acetone soaking time, the value is 10-20h, a is the correction coefficient, the value is 0.31-0.35, W1 is the weight ratio of the quassia particles to the acetone, and W2 is the weight ratio of the quassia particles to the absolute ethyl alcohol.
In some preferred embodiments of the present invention, in S06, the pressure control of the nano collider pulverizing is raised to the target pressure by the following PID control algorithm:
wherein, the delta u (c) corresponds to the variation of the pressure in the time interval of two times of testing pressure; kc is a constant, 12-14; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.5-2.0 s; TD is differential time, 1.5-2.0 min; TI is integration time, 1.5-2 min.
The invention has the beneficial effects that:
(1) the preparation method of the nano-scale traditional Chinese medicine powder obtains the nano-scale powder of the traditional Chinese medicine quassia.
(2) The preparation method of the nano-scale traditional Chinese medicine powder disclosed by the invention finds the unexpected technical effect of the steps of pretreatment and low-temperature control of acetone and absolute ethyl alcohol.
(3) The preparation method of the nano-scale traditional Chinese medicine powder also discovers the influence of lecithin as a specific surfactant on the action of the nano collider.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless otherwise specified, the examples and comparative examples are parallel tests with the same components, component contents, preparation steps, preparation parameters.
Example 1
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding acetone with the weight ratio of 5 times, soaking for 14 hours, and drying; adding 5 times of anhydrous ethanol, soaking for 5h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) the suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 6 particles in the nanometer range are contained in each 10 particles.
Example 2
Preparation method of nano-scale traditional Chinese medicine powder
(1) After washing the quassia tree with clear water, drying the quassia tree with a dryer and carrying out primary chopping on the quassia tree with a rotary crusher until the particle size is about 450 mu m.
(2) Adding acetone with the weight ratio of 6 times, soaking for 12 hours, and drying; adding 4 times of anhydrous ethanol, soaking for 6h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 40 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) treating with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particles into suspension of less than 10 μm, the ultrasonic pulverizing time is 35 minutes, and pulverizing power is 650W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) the suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 6 particles of the nanometer size were present per 10 particles, corresponding to example 1.
Example 3
Preparation method of nano-scale traditional Chinese medicine powder
(1) The quassia is washed with clear water, dried by a dryer and primarily cut up by a rotary crusher to a particle size of about 550 μm.
(2) Adding acetone with the weight ratio of 4 times, soaking for 16h, and drying; adding absolute ethyl alcohol with the weight ratio of 6 times, soaking for 4 hours, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 55 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 55 minutes, the pulverizing power is 500W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) the suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 6 particles of the nanometer size were present per 10 particles, corresponding to example 1.
Example 4
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding acetone with the weight ratio of 5 times, soaking for 14 hours, and drying; adding 5 times of anhydrous ethanol, soaking for 5h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) filtering the suspension with 300 mesh filter screen, collecting filtrate, and adding lecithin at a ratio of 0.1g per 100 ml. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 8 particles of the nanometer size are present in each 10 particles. The performance is obviously better than that of the embodiment 1, and P is less than 0.05.
Example 5
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding acetone with the weight ratio of 5 times, soaking for 14 hours, and drying; adding 5 times of anhydrous ethanol, soaking for 5h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) filtering the suspension with 300 mesh filter screen, collecting filtrate, and adding lecithin at a ratio of 0.01g per 100 ml. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 7 particles of the nanoscale are present in each 10 particles. This corresponds to example 1.
Example 6
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding acetone with the weight ratio of 5 times, soaking for 14 hours, and drying; adding 5 times of anhydrous ethanol, soaking for 5h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(4) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(5) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(6) filtering the suspension with 300 mesh filter screen, collecting filtrate, and adding lecithin at a ratio of 0.5g per 100 ml. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
The particles of nanometer order are most observed by a scanning electron microscope. At least 6 particles of the nanometer size were present per 10 particles, corresponding to example 1.
Example 7
Preparation method of nano-scale traditional Chinese medicine powder
The difference from example 1 is that in S02, the time T2 for the absolute ethanol soak was determined by the following formula:
wherein T1 is the acetone soaking time, the value is 10-20h, a is the correction coefficient, the value is 0.31-0.35, W1 is the weight ratio of the quassia particles to the acetone, and W2 is the weight ratio of the quassia particles to the absolute ethyl alcohol.
The determination of the soaking time of the absolute ethyl alcohol in the embodiment can obtain the quassia powder with high nanoscale proportion, and the soaking time of the absolute ethyl alcohol can be rapidly and effectively determined.
Example 8
Preparation method of nano-scale traditional Chinese medicine powder
The difference from example 1 is that, in S06, the pressure control of the nano collider pulverization is raised to the target pressure by the following PID control algorithm:
wherein, the delta u (c) corresponds to the variation of the pressure in the time interval of two times of testing pressure; kc is a constant, 12-14; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.5-2.0 s; TD is differential time, 1.5-2.0 min; TI is integration time, 1.5-2 min.
The pressure control method of the embodiment has the advantages of fast and stable pressure rise value and small variation fluctuation, and lays a good foundation for the nano-scale preparation of the quassia powder.
Comparative example 1
Preparation method of nano-scale traditional Chinese medicine powder
The method of CN1672720A is adopted to treat ramulus Et folium Picrasmae, i.e. after rinsing with clear water, drying with a drier and primarily cutting with a rotary grinder to a particle size of about 500 μm. Adding water at the weight ratio of picrasma quassioides to water of 1: 50 to obtain picrasma quassioides suspension. Pulverizing ramulus Et folium Picrasmae into suspension with particle size less than 10 μm by ultrasonic pulverizing at 600W for 40 min. The suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, and processing at 130Mpa and 300rpm for 2 h.
The scanning electron microscope showed almost no particles of nanometer order. The number of nano-sized particles is less than 2 per 10 particles.
Comparative example 2
Preparation method of nano-scale traditional Chinese medicine powder
The difference from comparative example 1 is that the crushing treatment time of the nano collider was extended to 5 hours.
Similar to comparative example 1, there were almost no nano-sized particles. The number of nano-sized particles is less than 2 per 10 particles.
Comparative example 3
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(3) controlling the temperature of the picrasma quassioides suspension to be below 2 ℃ by using an ice bath;
(4) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
(5) the suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
Similar to comparative example 1, there were almost no nano-sized particles. The number of nano-sized particles is less than 2 per 10 particles.
Comparative example 4
Preparation method of nano-scale traditional Chinese medicine powder
(1) Washing ramulus Et folium Picrasmae with clear water, drying with a drier, and primarily cutting with a rotary pulverizer to obtain particles with a size of about 500 μm.
(2) Adding acetone with the weight ratio of 5 times, soaking for 14 hours, and drying; adding 5 times of anhydrous ethanol, soaking for 5h, and drying;
(3) adding water in the weight ratio of picrasma quassioides to water of 1 to 50 to obtain picrasma quassioides suspension;
(4) processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension of less than 10 μm, the time of ultrasonic pulverization is 40 minutes, the pulverizing power is 600W; the temperature is not controlled in the whole process, and the temperature of the suspension system can be increased to 30 ℃ (about 5 ℃ higher than room temperature);
(5) the suspension was filtered through a 300 mesh sieve and the filtrate was collected. Pulverizing with a nanometer collider, processing at 130Mpa pressure and 300rpm for 2h, and observing with a scanning electron microscope.
Similar to comparative example 1, there were almost no nano-sized particles. The number of nano-sized particles is less than 2 per 10 particles.
Comparative example 6
Preparation method of nano-scale traditional Chinese medicine powder
The difference from example 4 is that tween 80 is used instead of lecithin.
Similar to example 4, the nanometer-sized particles dropped significantly, about 6, per 10 particles.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. A preparation method of nano-scale quassia powder is characterized by comprising the following steps:
s01, cleaning the quassia, drying and crushing;
s02, pretreating with acetone and absolute ethyl alcohol, and drying;
s03, preparing quassia water suspension;
s04, cooling;
s05, processing by an ultrasonic pulverizer;
s06, filtering, and crushing the filtrate by using a nano collider;
s07, drying to obtain nanometer Chinese medicinal powder;
in S01, the pulverization is carried out by primary chopping to a particle size of 450-;
s02, soaking in acetone, drying, soaking in absolute ethyl alcohol, and drying;
in S04, controlling the temperature of the quassia suspension to be below 2 ℃;
in S05, processing with ultrasonic pulverizer to pulverize ramulus Et folium Picrasmae particle into suspension less than 10 μm; controlling the temperature to be below 2 ℃ by using an ice bath in the whole process;
in S06, filtering with 300 mesh sieve, collecting filtrate, pulverizing with nanometer collider, and treating at 130MPa pressure and 300rpm for 2 hr.
2. The preparation method according to claim 1, wherein in S02, acetone in an amount of 4-6 times by weight is added, soaked for 12-16h, and dried; adding 4-6 times of anhydrous alcohol, soaking for 4-6 hr, and drying.
3. The process according to claim 1 or 2, wherein in S03, the weight ratio of quassia to water in the aqueous suspension of quassia is 1: 40-55.
4. The method according to claim 1 or 2, wherein the time T2 of the soaking in anhydrous ethanol in S02 is determined by the following formula:
wherein T1 is the acetone soaking time, the value is 10-20h, a is the correction coefficient, the value is 0.31-0.35, W1 is the weight ratio of the quassia particles to the acetone, and W2 is the weight ratio of the quassia particles to the absolute ethyl alcohol.
5. The production method according to claim 1 or 2, wherein in S06, the pressure control of the nano collider pulverization is raised to a target pressure by the following PID control algorithm:
wherein, the delta u (c) corresponds to the variation of the pressure in the time interval of two times of testing pressure; kc is a constant, 12-14; f (C) is the deviation at the time of sampling C, f (C-1) is the deviation at the time of sampling C-1, and f (C-2) is the deviation at the time of sampling C-2; TS is sampling period, 1.5-2.0 s; TD is differential time, 1.5-2.0 min; TI is integration time, 1.5-2 min.
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| CN1672720A (en) * | 2004-03-25 | 2005-09-28 | 香港理工大学 | Prepn process of Chinese medicine nano prepn |
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| CN1672720A (en) * | 2004-03-25 | 2005-09-28 | 香港理工大学 | Prepn process of Chinese medicine nano prepn |
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