CN114848600B - Fresh motherwort traditional Chinese medicine formula granule and preparation method thereof - Google Patents
Fresh motherwort traditional Chinese medicine formula granule and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of fresh motherwort formula particles, which comprises the following steps: obtaining fresh motherwort decoction pieces; mixing the fresh motherwort decoction pieces with boiling water, and decocting to prepare fresh motherwort extract; filtering the fresh motherwort extract, concentrating the filtrate, and preparing fresh motherwort extract; mixing the fresh motherwort extract with auxiliary materials, drying and granulating. The preparation method has high yield, low cost, high content of effective components in the prepared fresh motherwort granule, and high safety.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine preparations, in particular to a fresh motherwort traditional Chinese medicine formula granule and a preparation method thereof.
Background
Fresh motherwort is a fresh overground part of a Labiatae plant, namely Leonurus japonicus Houtt, is harvested from a seedling stage in spring to a early stage of early summer flowers, is slightly cold in nature, bitter and pungent in taste, has the effects of activating blood and regulating menstruation, promoting urination and detumescence, clearing heat and detoxicating, is clinically commonly used for treating irregular menstruation, dysmenorrhea amenorrhea, lochiorrhea, edema and oliguria, pyocutaneous disease and toxic swelling and other symptoms, is known as a "gynecological essential drug", and is a fresh medicinal material commonly used in traditional Chinese medicine.
The main chemical components of the fresh motherwort comprise various components such as alkaloids, flavonoids, terpenes, phenethyl alcohol glycoside, volatile oil and the like, wherein the alkaloids and the flavonoids are substances which mainly exert the drug effect. Studies show that stachydrine and leonurine have remarkable pharmacological activity on uterus and heart, leonurine water-soluble alkaloids and total flavonoids have excitation effect on the uterus of mice in vitro, and fat-soluble alkaloids have inhibition effect on the uterus of mice in vitro. In addition, alkaloid and flavone components in the motherwort can also effectively inhibit myocardial tissue ischemia injury caused by Isoprenaline (ISO).
At present, the common motherwort preparation in clinic comprises motherwort capsules, motherwort fluid extracts, motherwort tablets and the like, and the used materials are mainly dry motherwort, but the dry motherwort products and fresh motherwort products are greatly different and cannot be mixed. The content measurement items of motherwort in the content assembly of the new and revised version (one part) of the edition 2000 of Chinese pharmacopoeia are as follows: the product contains alkaloid and stachydrine hydrochloride (C 7 H 13 NO 2 HCl) and not less than 0.40% of dry product and not less than 1.0% of fresh product. It can be seen that stachydrine hydrochloride in fresh herba Leonuri is 2 times that in dry product. Meanwhile, researches show that after fresh motherwort is dried, various components such as alkaloid (stachydrine and leonurine) and flavone (rutin, quercetin, apigenin and genkwanin) change to different degrees, wherein the content of stachydrine hydrochloride and leonurine hydrochloride is reduced by nearly one time, the content of rutin, quercetin and genkwanin is also reduced, and the content of apigenin is increased after being dried. In addition, the harvesting period of fresh motherwort is different from that of dry motherwort, and the fresh product is the spring seedling stageHarvesting and cutting in early stage of early summer flowers; the dry product is obtained by cutting when the stem and leaf are luxuriant in summer and the flower is not opened or is opened initially, and the total alkaloid content gradually decreases from seedling stage to flowering to mature fruit in the whole growth process of the motherwort. Meanwhile, under the same dosage, the drug effect of the motherwort in different growth periods is different, and the in-vitro uterine contraction effect of the motherwort in different growth periods on rats is sequentially from strong to weak and is fresh in the early stage of flowers>Bud stage>Full bloom stage. Thus, the fresh motherwort is greatly different from the dry motherwort.
The traditional method prepares the fresh motherwort powder through the steps of cleaning, chopping, juicing, decompressing and concentrating and freeze-drying, but the obtained juice is less, the yield is low after the squeezing, the cost of the product is increased, and the microbial index is easily disqualified, so that the safety of medication is difficult to ensure.
Still another conventional method is by crushing fresh herba Leonuri, pulping, squeezing to obtain juice, adding appropriate amount of water into the residue, mixing, squeezing, repeating for 2-3 times, mixing the juices, filtering, concentrating, and spray drying. The preparation method can enable the components to flow out by breaking cell walls, and solves the problem of administration of fresh motherwort to a certain extent, but the finally prepared fresh motherwort particles still have the problems of low content of various effective components and low transfer rate.
Disclosure of Invention
Based on the above, it is necessary to provide a preparation method of fresh motherwort herb formula particles, which has high yield, low cost, high content of active ingredients of the prepared fresh motherwort herb formula particles and high safety.
The invention is realized by the following technical scheme.
A preparation method of fresh motherwort formula particles comprises the following steps:
obtaining fresh motherwort decoction pieces;
mixing the fresh motherwort decoction pieces with boiling water, and decocting to prepare fresh motherwort extract;
filtering the fresh motherwort extract, concentrating the filtrate, and preparing fresh motherwort extract;
mixing the fresh motherwort extract with auxiliary materials, drying and granulating.
In one embodiment, the number of times of decoction is 1 to 3 times.
In one embodiment, in each decoction, the mass ratio of the fresh motherwort decoction pieces to the boiling water is respectively and independently selected from 1 (5-18).
In one embodiment, the time of each decoction is independently selected from 0.5h to 2h.
In one embodiment, the preparation of the fresh motherwort decoction pieces comprises the following steps:
removing impurities from fresh herba Leonuri plants, cleaning, removing surface water, cutting, and standing;
wherein the specification of the cut sections is 0.5 cm-2 cm.
In one embodiment, the time to wait is within 4 hours.
In one embodiment, the conditions of concentration include: concentrating under reduced pressure at 40-80 deg.c to obtain fluid extract with relative density of 1.02-1.20.
In one embodiment, the method of drying is selected from one or both of freeze drying and spray drying.
In one embodiment, the auxiliary material is selected from one or more of maltodextrin, dextrin, starch, lactose, silicon dioxide and magnesium stearate.
The invention also provides fresh motherwort formula particles prepared by the preparation method of the fresh motherwort formula particles.
Compared with the prior art, the preparation method of the fresh motherwort formula particle has the following beneficial effects:
the preparation method of the fresh motherwort formula granule adopts a decoction extraction process and a concentration process, so that the content of active ingredients of the fresh motherwort is obviously improved, including leonurine hydrochloride, stachydrine hydrochloride and the like, the yield can be effectively improved, and the cost is reduced. Meanwhile, the invention uses water as solvent for extraction in the process of decoction, the usage is safer, the traditional medicine theory of traditional Chinese medicine is met, and the boiling water feeding process can further improve the content and the yield of the active ingredients. In addition, the water decoction step also greatly improves the microorganism qualification probability of the obtained fresh motherwort extract, and ensures the safety of clinical medication of the fresh medicine.
Furthermore, the fresh motherwort traditional Chinese medicine formula granule prepared by the preparation method of the fresh motherwort traditional Chinese medicine formula granule can maintain the original curative effect and characteristics of decoction, is convenient to carry and take, is convenient to store and has small dosage.
Drawings
FIG. 1 is a schematic diagram of a preparation flow of fresh motherwort formula particles provided by the invention;
FIG. 2 is a comparison feature map provided by the present invention; wherein, peak 1 represents new chlorogenic acid, peak 3 represents chlorogenic acid, peak 6 represents leonurine hydrochloride, and peak 8 represents rutin.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. The drawings illustrate preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise. In the description of the present invention, the meaning of "several" means at least one, such as one, two, etc., unless specifically defined otherwise.
The words "preferably," "more preferably," and the like in the present invention refer to embodiments of the invention that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values for the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, the invention provides a preparation method of fresh motherwort formula particles, which comprises the following steps:
obtaining fresh motherwort decoction pieces;
mixing fresh herba Leonuri decoction pieces with boiling water, and decocting to obtain fresh herba Leonuri extractive solution;
filtering the fresh herba Leonuri extractive solution, concentrating the filtrate, and preparing into fresh herba Leonuri fluid extract;
mixing fresh herba Leonuri fluid extract with adjuvants, drying, and granulating.
The traditional Chinese medicine formula granule is prepared by extracting single traditional Chinese medicine decoction pieces with water, concentrating, drying and granulating, is taken by patients according to the traditional Chinese medicine clinical prescription under the guidance of the traditional Chinese medicine theory, has the clinical curative effect consistent with that of the corresponding decoction pieces, has the advantages of no need of decoction, small dosage, convenient carrying and the like, and the fresh motherwort is prepared into the fresh motherwort formula granule, so that the characteristics of fresh medicines are reserved, the extraction of active ingredients is more complete, the loss is reduced, and the production cost is reduced.
The boiling water feeding process can obviously improve the content of active ingredients, effectively improve the yield and reduce the cost.
In a specific example, the number of times of decoction is 1 to 3 times.
In a specific example, in each decoction, the mass ratio of the fresh motherwort decoction pieces to the boiling water is respectively and independently selected from 1 (5-18).
It will be appreciated that in the present invention, the mass ratio of fresh motherwort pieces to boiling water in each decoction includes, but is not limited to, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:14, 1:16, 1:18.
In a specific example, the time of each decoction is independently selected from 0.5h to 2h.
It is understood that in the present invention, the time of each decoction includes, but is not limited to, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1.0h, 1.1h, 1.2h, 1.5h, 2h.
In a specific example, the preparation of the fresh motherwort decoction pieces comprises the following steps:
removing impurities from fresh herba Leonuri plants, cleaning, removing surface water, cutting, and standing;
wherein the specification of the cut sections is 0.5 cm-2 cm.
It is understood that the specifications of the cut segments include, but are not limited to, 0.5cm, 0.6cm, 0.7cm, 0.8cm, 0.9cm, 1cm, 1.2cm, 1.4cm, 1.6cm, 1.8cm, 2cm.
It will be appreciated that in the present invention, waiting refers to waiting for the time for the next process.
In a specific example, the material to be cut is placed in air at room temperature.
In one specific example, the time to wait is within 4 hours. It is understood that the time to wait includes, but is not limited to, 0h, 1h, 2h, 3h, 4h.
The fresh motherwort decoction pieces have obvious change trend in the material waiting process, so that the total ingredients in the fresh motherwort formula particles are kept as much as possible, and the material waiting time is controlled within 4 hours.
In one specific example, the conditions of concentration include: concentrating under reduced pressure at 40-80 deg.c to obtain fluid extract with relative density of 1.02-1.20.
The invention adopts vacuum low-temperature concentration in the concentration process, reduces the heating time of heat-sensitive components, further effectively avoids the inactivation of the components and improves the medicinal value of the product.
In a specific example, the method of drying is selected from one or both of freeze drying and spray drying.
In a specific example, the adjunct is selected from maltodextrin.
In a specific example, the granulation is dry granulation.
Preferably, the preparation method of the fresh motherwort formula particles comprises the following steps:
obtaining fresh motherwort decoction pieces;
mixing fresh motherwort decoction pieces with boiling water, and decocting for 1-3 times to prepare fresh motherwort extract; wherein, in each decoction, the mass ratio of the fresh motherwort decoction pieces to the boiling water is respectively and independently selected from 1 (5-18); and/or the time of each decoction is respectively and independently selected from 0.5 to 2 hours;
filtering the fresh motherwort extract, concentrating the filtrate under reduced pressure at the temperature of 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, and preparing fresh motherwort fluid extract;
mixing fresh herba Leonuri fluid extract with adjuvants, drying, and granulating.
In a more specific example, the preparation method of the fresh motherwort formula granule comprises the following steps:
pretreatment: taking fresh motherwort plants, removing impurities, cleaning, and cutting into segments to obtain fresh motherwort decoction pieces; wherein the specification of the cut sections is 0.5 cm-2 cm;
extracting: decocting fresh motherwort decoction pieces in boiling water for 1-3 times, 5-18 times of water each time, and 0.5-2 hours, and combining to obtain fresh motherwort extract;
concentrating: filtering the extracting solution, concentrating the filtrate under reduced pressure at the temperature of 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thus obtaining fresh motherwort fluid extract;
and (3) drying: dissolving fresh herba Leonuri fluid extract with adjuvants, and drying to obtain fresh herba Leonuri dry extract powder;
granulating: and adding proper amount of auxiliary materials into the fresh motherwort dry paste powder, and performing dry granulation to obtain fresh motherwort formula granules.
The invention also provides fresh motherwort formula particles prepared by the preparation method of the fresh motherwort formula particles.
The following are specific examples, and all materials used in the examples are commercially available products unless otherwise specified.
Example 1
The embodiment provides a preparation method of fresh motherwort grains, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. decocting the fresh herba Leonuri in water twice, adding 10 times of water for the first time, heating to boil, adding decoction pieces, and decocting for 1.0 hr; adding water with the dosage of 8 times for the second time, heating to boil, decocting for 0.5h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain fresh herba Leonuri extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort clear paste (sieving with 120-250 mesh sieve), adding proper amount of auxiliary materials, dissolving, and spray drying to obtain fresh motherwort dry paste powder;
e. taking fresh motherwort dry extract powder, adding a proper amount of auxiliary materials, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Example 2
The embodiment provides a preparation method of fresh motherwort grains, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. decocting the fresh herba Leonuri in water twice, adding 10 times of water for the first time, heating to boil, adding decoction pieces, and decocting for 1.0 hr; adding water with the dosage of 8 times for the second time, heating to boil, decocting for 0.5h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain fresh herba Leonuri extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort clear paste (sieving with 120-250 mesh sieve), adding proper amount of auxiliary materials, dissolving, and freeze-drying to obtain fresh motherwort dry paste powder;
e. taking fresh motherwort dry extract powder, adding a proper amount of auxiliary materials, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Example 3
The embodiment provides a preparation method of fresh motherwort grains, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. taking fresh motherwort after being cut into sections, adding 18 times of water into the fresh motherwort, heating to boiling, adding decoction pieces, decocting for 1.0h, and filtering (sieving with a 120-400 mesh sieve) to obtain a fresh motherwort extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort extract, adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain fresh motherwort dry extract powder;
e. and (3) taking fresh motherwort dry paste powder, adding a proper amount of maltodextrin, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Example 4
The embodiment provides a preparation method of fresh motherwort grains, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into sections of 2cm;
b. decocting the fresh herba Leonuri in water twice, adding 9 times of water for the first time, heating to boil, adding decoction pieces, and decocting for 1.0 hr; adding 7 times of water, heating to boil, decocting for 0.5h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain fresh herba Leonuri extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort extract, adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain fresh motherwort dry extract powder;
e. and (3) taking fresh motherwort dry paste powder, adding a proper amount of maltodextrin, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Example 5
The embodiment provides a preparation method of fresh motherwort grains, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. decocting the fresh herba Leonuri in water twice, adding 12 times of water for the first time, heating to boil, adding decoction pieces, and decocting for 1.0 hr; adding water with the dosage of 10 times for the second time, heating to boiling, decocting for 1.0h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain fresh herba Leonuri extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort extract, adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain fresh motherwort dry extract powder;
e. and (3) taking fresh motherwort dry paste powder, adding a proper amount of maltodextrin, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Comparative example 1
The comparative example provides a preparation method of dry motherwort granules, which comprises the following steps:
a. taking dry herba Leonuri decoction pieces, removing impurities, and cutting into 1cm sections;
b. decocting herba Leonuri in water twice, adding decoction pieces, adding 9 times of water, heating to boiling, and decocting for 1.0 hr; adding 7 times of water, heating to boil, decocting for 0.5h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain herba Leonuri extract;
c. concentrating the motherwort extractive solution at 40-80deg.C under reduced pressure to obtain fluid extract with relative density of 1.02-1.20;
d. filtering herba Leonuri fluid extract (sieving with 120-250 mesh sieve), adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain herba Leonuri dry extract powder;
e. and (3) adding a proper amount of maltodextrin into the motherwort dry extract powder, granulating by a dry method, and packaging to obtain motherwort granules.
Comparative example 2
The comparative example provides a preparation method of fresh motherwort (juice) formula granules, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. crushing the fresh motherwort after being cut into segments by a coarse crusher, pulping, squeezing juice, adding a proper amount of water into residues, uniformly mixing and squeezing juice, repeating for 2-3 times, merging the juice, and filtering to obtain fresh motherwort juice;
c. concentrating fresh motherwort juice under reduced pressure at 55-65 ℃ until the relative density is 1.02, thus obtaining fresh motherwort concentrated juice;
d. filtering fresh motherwort concentrated juice (sieving with 120-250 mesh sieve), adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain "dry motherwort extract powder";
e. and (3) adding a proper amount of maltodextrin into the motherwort dry paste powder, granulating by a dry method, and packaging to obtain fresh motherwort (juice) formula granules.
Comparative example 3
The comparative example provides a preparation method of fresh motherwort formula particles, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. decocting fresh herba Leonuri in water (at room temperature) twice, adding decoction pieces, adding water (at room temperature) 10 times of the amount of the materials, heating to boiling, and decocting for 1.0 hr; adding water (normal temperature) with the dosage of 8 times for the second time, heating to boiling, decocting for 0.5h, mixing decoctions, and filtering (sieving with 120-400 mesh sieve) to obtain fresh herba Leonuri extract;
c. concentrating the fresh motherwort extract under reduced pressure at 40-80 ℃ to obtain fluid extract with the relative density of 1.02-1.20, thereby obtaining fresh motherwort fluid extract;
d. filtering fresh motherwort extract, adding appropriate amount of maltodextrin, dissolving, and spray drying to obtain fresh motherwort dry extract powder;
e. and (3) taking fresh motherwort dry paste powder, adding a proper amount of maltodextrin, granulating by a dry method, and packaging to obtain fresh motherwort granules.
Comparative example 4
The comparative example provides a method for investigating the waiting time of fresh motherwort decoction pieces, which comprises the following steps:
a. removing impurities from the fresh collected motherwort plants, cleaning, draining off surface water, and cutting into 1cm sections;
b. and (3) taking the cut decoction pieces, and respectively placing the decoction pieces for 0, 2, 4 and 6 hours at normal temperature to obtain the fresh motherwort decoction pieces.
Effect verification experiment
The extract yield, index component content, characteristic spectrum, microbial condition of the motherwort grains of examples 1 to 5 and comparative examples 1 to 3 and the index component content and characteristic spectrum of the fresh motherwort decoction pieces of comparative example 4 were measured.
The method for measuring the paste yield comprises the following steps:
reference is made to the method under the water-soluble extract assay (general rule 2201 of the chinese pharmacopoeia 2020 edition). The specific method is that 25mL of filtrate is precisely measured, the filtrate is placed in an evaporation dish M1 which is dried to constant weight, and after being evaporated to dryness in a water bath, the filtrate is dried for 3 hours at 105 ℃, and the filtrate is cooled for 30 minutes in a dryer, so that the weight M2 is rapidly and precisely weighed. The feeding amount of the decoction pieces is M, the volume of the extracting solution is V, and the calculation formula of the paste yield is as follows:
the measuring method of the content of the index component comprises the following steps:
leonurine hydrochloride: reference is made to high performance liquid chromatography (rule 0512 of the edition of chinese pharmacopoeia 2020).
The chromatographic condition and system applicability test uses octadecylsilane chemically bonded silica as filler; acetonitrile-0.4% sodium octane sulfonate 0.1% phosphoric acid solution (24:76) is used as mobile phase; the detection wavelength was 277nm. The theoretical plate number is not less than 6000 according to the leonurine hydrochloride peak.
Stachydrine hydrochloride: reference is made to high performance liquid chromatography (rule 0512 of the edition of chinese pharmacopoeia 2020).
The chromatographic condition and system applicability test uses propyl amide bonded silica gel as filler; acetonitrile-0.2% glacial acetic acid solution (80:20) is taken as a mobile phase; detected with an evaporative light scattering detector. The theoretical plate number is not less than 6000 calculated according to the hydrochloric acid water Su Jianfeng.
The measuring method of the characteristic map comprises the following steps:
reference is made to high performance liquid chromatography (rule 0512 of the edition of chinese pharmacopoeia 2020).
Octadecylsilane chemically bonded silica is used as filler (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); acetonitrile is taken as a mobile phase A, a 0.1% phosphoric acid aqueous solution is taken as a mobile phase B, and the gradient elution procedure is as follows: 0-11 min,3% -10% (A), 97% -90% (B); 11-15 min,10% -11% (A), 90% -89% (B); 15-22 min,11% -12% (A), 89% -88% (B); 22-28 min,12% -16% (A), 88% -84% (B); 28-30 min,16% -20% (A), 84% -80% (B); 30-34 min,20% -22% (A), 80% -78% (B); 34-40 min,22% -60% (A), 78% -40% (B); 40-41 min,60% -3% (A), 40% -97% (B); 41-50 min,3% -97% (A), 97% -3% (B); the flow rate was 0.25mL per minute; the column temperature is 30 ℃; the detection wavelength was 277nm.
The chromatogram of the sample should show 8 characteristic peaks, wherein 4 peaks should respectively correspond to the retention time of the corresponding reference peaks of the reference substance; the peak corresponding to the chlorogenic acid reference peak is the S1 peak, the relative retention time of the characteristic peak 2 and the S1 peak is calculated, the relative retention time is within +/-10% of the specified value, and the specified value is: 0.90 (Peak 2); the peak corresponding to the leonurine hydrochloride reference peak is an S2 peak, the relative retention time of the characteristic peak 4, the peak 5, the peak 7 and the S2 peak is calculated, the relative retention time is within +/-10% of a specified value, and the specified value is: 0.94 (Peak 4), 0.97 (Peak 5), 1.19 (Peak 7). The contrast characteristic map of fresh herba Leonuri is shown in figure 2.
The method for measuring the microbial condition comprises the following steps: microbial limit inspection with reference to non-sterile product: microbiological count and control bacterial examination (China pharmacopoeia 2020 edition general rules 1105-1106).
The results of investigation of the preparation methods and parameters, the paste yield, the index component content, the peak areas of the characteristic patterns and the microbial conditions of examples 1 to 5 and comparative examples 1 to 3 are shown in Table 1, wherein the ratio of the sampling amount of the characteristic patterns of example 1 to comparative example 1 is 1:2.
TABLE 1
As can be seen from examples 1-5, the active ingredients (leonurine hydrochloride and stachydrine hydrochloride) of the fresh motherwort granule prepared by the method have higher content, and the detection of microorganisms is qualified.
Example 1 is different from examples 2 to 5 in that the parameters such as the decoction piece size, the number of times of decoction, the time, the water addition amount and the like are different, and the above parameters have a certain influence on the content of the active ingredient.
Comparative example 1 is prepared directly from dry motherwort decoction pieces, and comparative example 1 shows that the fresh motherwort particles in example 1 have larger differences from the motherwort formula particles in terms of paste yield, index component content and characteristic spectrum, the paste yield differs by about 1.5 times, the content of leonurine hydrochloride and stachydrine hydrochloride differs by about 2-3 times, the characteristic spectrum also shows obvious differences, and under the condition that the sampling amount of the dry motherwort particles is doubled, the peak areas of novel chlorogenic acid, peak 2, chlorogenic acid, peak 5, peak 7 and rutin in the characteristic spectrum are still obviously lower than those of the fresh motherwort particles, and the peak area of rutin with the largest difference is 3.5 times, so that the fresh motherwort particles prepared by the invention are obviously different from the motherwort formula particles in the market at present.
In comparison with example 1, comparative example 2 uses a process of squeezing juice with chilled water and concentrating at 55 to 65 ℃. As can be seen from Table 1, the fresh motherwort particles prepared by the water extraction process in example 1 are significantly higher in both paste yield and content of leonurine hydrochloride and stachydrine hydrochloride than the particles prepared by juicing, and the peak area of the characteristic spectrum of the water extraction process is also larger than that of the juice, and in addition, the conditions that the total number of aerobic colonies and the microbial indexes of mold and yeast are out of the specified limits occur due to the low temperature and lack of effective sterilization technology in the whole preparation process of comparative example 3. The invention can extract the effective components of the fresh motherwort to the maximum extent, thereby ensuring the clinical efficacy of the fresh motherwort, and simultaneously can strictly control the microorganism of the product, solve the problem of unqualified microorganism of the fresh medicine preparation and ensure the safety of the clinical medicine application of the fresh medicine.
Comparative example 3 was cold water extracted in a conventional manner as compared to example 1. As can be seen from Table 1, the extract yield and index component content of the fresh motherwort granule prepared by the boiling water extraction process in example 1 are obviously higher than those of the fresh motherwort granule prepared by the cold water extraction, the peak areas of the characteristic spectrum of the boiling water extraction are also improved to different degrees compared with those of the fresh motherwort granule prepared by the cold water extraction, and the total peak areas are improved by more than 15%, so that the content of each component in the fresh motherwort granule can be obviously improved by adopting the boiling water extraction mode.
The measurement results of the index component content of the fresh motherwort decoction piece of comparative example 4 and the peak areas of the characteristic patterns are shown in Table 2.
TABLE 2
From Table 2, the fresh motherwort decoction pieces have obvious change trend in the process of waiting for materials, the components of the leonurine hydrochloride and the stachydrine hydrochloride are increased, and the peak areas of the peak 7 and the rutin are obviously reduced. In order to control the total components in the fresh motherwort prescription granule to be kept as much as possible, the waiting time should be controlled within 4 hours.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the fresh motherwort formula granule is characterized by comprising the following steps of:
removing impurities from fresh motherwort plants, cleaning, removing surface water, cutting into sections, and obtaining fresh motherwort decoction pieces when materials are prepared; the time for waiting for the material is within 4 hours;
mixing the fresh motherwort decoction pieces with boiling water, and decocting to prepare fresh motherwort extract;
filtering the fresh motherwort extract, concentrating the filtrate, and preparing fresh motherwort extract; the conditions of the concentration include: concentrating under reduced pressure at 40-80 deg.c to obtain fluid extract with relative density of 1.02-1.20;
mixing the fresh motherwort extract with auxiliary materials, drying and granulating.
2. The method for preparing fresh motherwort herb granules according to claim 1, wherein the number of times of decoction is 1 to 3.
3. The preparation method of the fresh motherwort formula particles according to claim 2, wherein the mass ratio of the fresh motherwort decoction pieces to boiling water in each decoction is respectively and independently selected from 1 (5-18).
4. The method for preparing fresh motherwort herb granules according to claim 2, wherein the time of each decoction is independently selected from 0.5 to 2 hours.
5. The preparation method of the fresh motherwort formula particles according to claim 1, which is characterized in that,
the specification of the cut sections is 0.5 cm-2 cm.
6. The method for preparing fresh motherwort formulation granule according to claim 1, wherein the drying method is one or both of freeze-drying and spray-drying.
7. The method for preparing fresh motherwort formula particles according to claim 1, wherein the auxiliary materials are selected from one or more of maltodextrin, dextrin, starch, lactose, silicon dioxide and magnesium stearate.
8. The method for preparing fresh motherwort formulation granules according to claim 7, wherein said auxiliary material is selected from maltodextrin.
9. The method of claim 1, wherein the granulating is dry granulating.
10. A fresh motherwort granule prepared by the preparation method of the fresh motherwort granule according to any one of claims 1 to 9.
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| CN1456257A (en) * | 2003-02-20 | 2003-11-19 | 毛友昌 | Fresh motherwort particle preparing method |
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| CN110123907A (en) * | 2019-06-21 | 2019-08-16 | 广东一方制药有限公司 | A kind of flavour amino acid granule and preparation method thereof |
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| CN1456257A (en) * | 2003-02-20 | 2003-11-19 | 毛友昌 | Fresh motherwort particle preparing method |
| CN102058661A (en) * | 2010-01-20 | 2011-05-18 | 浙江大德药业集团有限公司 | Method for preparing fresh motherwort preparation |
| CN103933115A (en) * | 2014-04-01 | 2014-07-23 | 回音必集团安徽制药有限公司 | Motherwort granule preparation technology |
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