CN114917276A - Processing method of Heishun tablet - Google Patents

Processing method of Heishun tablet Download PDF

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CN114917276A
CN114917276A CN202210273064.3A CN202210273064A CN114917276A CN 114917276 A CN114917276 A CN 114917276A CN 202210273064 A CN202210273064 A CN 202210273064A CN 114917276 A CN114917276 A CN 114917276A
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soaking
water
time
content
monkshood
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陆兔林
高波
宫静雯
季德
张伟
毛春芹
薛蓉
屈凌芸
郭志俊
胡雨
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China Resources Sanjiu Modern Traditional Chinese Medicine Pharmaceutical Co ltd
Nanjing University of Chinese Medicine
Anhui China Resources Jinchan Pharmaceutical Co Ltd
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China Resources Sanjiu Modern Traditional Chinese Medicine Pharmaceutical Co ltd
Nanjing University of Chinese Medicine
Anhui China Resources Jinchan Pharmaceutical Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
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    • A61K36/71Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • A61K36/714Aconitum (monkshood)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting

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Abstract

The invention discloses a processing method of Heishun tablets, which comprises the following steps: cleaning radix Aconiti lateralis Preparata, soaking gallbladder, decocting, slicing, rinsing with water, dyeing, steaming in water, and drying; wherein, the appearance, the water-soluble extract, the content of monoester alkaloid and the content of diester alkaloid are used as evaluation indexes, the single-factor investigation is carried out on all variables, the parameter ranges of the gallbladder concentration, the gallbladder soaking time, the dyeing liquid proportion, the boiling time, the rinsing times, the steaming time and the drying temperature are determined, the orthogonal test is designed to determine the optimal process parameters, and the black and smooth slices are processed by utilizing the determined optimal process parameters. The invention changes the water bleaching after boiling in Chinese pharmacopoeia into cold soaking to room temperature by optimizing the processing technology; the processing technological parameters of the black tablets are definite, the processing technological process is standardized, and the existing quality standard evaluation is perfected. Compared with the traditional process, the method has the advantages of time saving, labor saving, standardization and better application prospect.

Description

Processing method of Heishun tablet
Technical Field
The invention belongs to the field of processing of traditional Chinese medicinal materials, and particularly relates to a processing technology of Heishun tablet decoction pieces.
Background
Radix Aconiti lateralis is processed from the root of Aconitum carmichaelii Debx of Ranunculaceae. Collected from late 6 to late 8 months, removed the mother root, fibrous root and silt, so called as Bufuzzi, with toxicity, modern researches show that Fu Zi has physiological activities of resisting arrhythmia, improving immunity, resisting inflammation and relieving pain. The processed product comprises salt aconite, black aconite, white aconite, light aconite and the like, wherein the black aconite is one of the clinical common specifications.
The traditional processing mode of the black flake is as follows: cleaning radix Aconiti lateralis Preparata, soaking in water solution of radix Aconiti lateralis Preparata for several days, decocting together with the soaking solution until it is thoroughly soaked, taking out, rinsing with water, longitudinally cutting into pieces with thickness of about 0.5cm, rinsing with water, dyeing the pieces with color matching solution to dark brown, taking out, steaming to oil level and luster, oven drying to semi-dry, and sun drying or oven drying.
At present, aiming at the processing of the Heishun tablet, the technological parameters of each link are fuzzy, and particularly, no specific regulation is made on the concentration days of gallbladder soaking and the time for boiling and steaming in the key steps. The traditional water bleaching process is defined as 'immersion bleaching overnight', so that the content loss of six alkaloids specified in a dictionary is large, and the technology and the operating procedure of the manufacturing and processing technology of the black shun tablets have no detailed standard, so that the quality of the black shun tablets is difficult to control, and the efficacy of the black shun tablets cannot be well exerted.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a black shun tablet processing device, which can save production time, improve production efficiency, define processing technological parameters of the black shun tablet, standardize processing technological process, improve the existing quality standard of the black shun tablet and ensure the quality of the black shun tablet.
In order to achieve the purpose, the invention adopts the following technical scheme:
a processing method of HEISHUN tablet comprises:
cleaning radix Aconiti lateralis Preparata, soaking gallbladder, decocting, slicing, rinsing with water, dyeing, steaming in water, and drying;
wherein, the process parameters are determined by the following method:
taking the appearance, the content of water-soluble extract, monoester alkaloid and diester alkaloid as evaluation indexes, carrying out single-factor investigation by taking the concentration of bile, the time for soaking bile, the boiling time, the number of times of water bleaching, the proportion of dyeing liquid, the steaming time and the drying temperature as variables, determining the concentration of bile, the time for soaking bile and the proportion of dyeing liquid, determining the parameter ranges of the boiling time, the number of times of water bleaching, the steaming time and the drying temperature, and designing an orthogonal test;
obtaining an experimental result of an orthogonal test, determining the influence degree of each factor by combining the visual analysis of the orthogonal test and the variance analysis, determining the optimal process parameters, and processing the black strips by using the determined optimal process parameters.
Preferably, the evaluation method of the appearance property is: and (4) grading the black and smooth slices from the aspects of color, texture and mouthfeel, and taking the total score as an index value of the appearance character.
Preferably, the determination mode of the concentration of the bile bar and the bile dunking time is as follows: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, then respectively putting the monkshood into the gallbladder solutions with different concentrations, observing the antiseptic effect of the solutions, obtaining the contents of the monoester alkaloid and the diester alkaloid after gallbladder soaking, taking the gallbladder solution without mould in 30 days as a premise, selecting the gallbladder soaking time which is appropriate and corresponds to the time when the ratio of the contents of the monoester alkaloid and the diester alkaloid is maximum as the middle time, and determining the gallbladder concentration and the gallbladder soaking time.
Preferably, the parameter range of the cooking time is determined in a manner that: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of bile and the time for soaking bile, boiling in a bile solution for different times respectively, observing the central character of the monkshood and obtaining the content of monoester alkaloid, selecting the boiling time which reaches the transparent standard specified in Chinese pharmacopoeia and has the highest content of the monoester alkaloid as the intermediate time, and determining the parameter range of the boiling time.
Preferably, the parameter range determining mode of the number of times of water rinsing is as follows: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing gallbladder concentration, gallbladder soaking time and boiling time, adding clear water for soaking after slicing, changing water for a soaking solution at a fixed frequency in the soaking process, investigating the content of calcium chloride and the content of ash and acid-insoluble ash in the soaking solution during each water change, selecting the soaking solution with the ash and acid-insoluble ash limit lower than that specified in Chinese pharmacopoeia, and selecting a water bleaching frequency range with proper water bleaching frequency and stable calcium chloride content.
Preferably, the method for determining the proportion of the staining solution comprises the following steps: taking a plurality of groups of cleaned aconite roots to remove fibrous root impurities, fixing the gallbladder concentration, the gallbladder soaking time and the boiling time, respectively soaking the sliced aconite roots in clear water, fixing the water changing times in the soaking process, soaking the sliced aconite roots in different dyeing solutions for dyeing, observing the appearance color of the dyed aconite roots, and determining the proportion of the dyeing solutions according to the color of the dark brown.
Preferably, the parameter range of the steaming time is determined in a manner that: removing fibrous root impurities from a plurality of groups of cleaned monkshood, fixing the concentration of bile, the time for soaking bile and the boiling time, slicing, respectively soaking in clear water, fixing the water changing times in the soaking process, soaking in dyeing solution with the same components for dyeing, then respectively steaming, timing from round gas, steaming for different times, observing the appearance of steamed monkshood, obtaining the content of monoester alkaloid and the content of diester alkaloid, selecting the steaming time which is lower than the limit of diester alkaloid specified in Chinese pharmacopoeia and has the highest content of monoester alkaloid as the middle time, and determining the parameter range of the steaming time.
Preferably, the parameter range of the drying temperature is determined in a manner that: removing fibrous root impurities from a plurality of groups of cleaned monkshood, fixing the concentration of bile, the time for soaking bile and the boiling time, slicing, respectively adding clear water for soaking, fixing the water changing times in the soaking process, soaking in dyeing solution with the same components for dyeing, fixing the steaming time, drying at different temperatures to obtain the content of monoester alkaloid and the content of diester alkaloid, selecting drying with the content of diester alkaloid lower than the limit specified in Chinese pharmacopoeia and the highest content of monoester alkaloid as intermediate time, and determining the parameter range of drying.
The invention also provides a processing method of the Heishun tablet, which comprises the following steps:
(1) bladder making: soaking the cleaned monkshood in a choline solution for 20 days, wherein the concentration of the choline solution is 30% (g/mL);
(2) boiling: decocting the soaked radix Aconiti lateralis and the gallbladder solution for 10min, and soaking to room temperature;
(3) slicing: slicing the monkshood obtained in the step (2) to obtain monkshood slices;
(4) rinsing with water: carrying out water rinsing on the monkshood slices, wherein water is changed for 4 times within 24 hours in the water rinsing process;
(5) dyeing: dyeing the rinsed monkshood slices with a dyeing solution; in the dyeing liquid, the mass ratio of brown sugar, water and rape oil is 1:1: 0.5;
(6) steaming: steaming the dyed radix Aconiti lateralis in a container for 3h after air circulation;
(7) and (3) drying: the steamed monkshood slices are dried for 6h at 65 ℃.
Preferably, the washing in step (1) is to wash the rhizoma acori graminei respectively according to size.
Preferably, the slicing in step (3) is performed by using a microtome.
Preferably, the slices in step (3) are cut to a thickness of 0.5 cm.
Preferably, the mass ratio of the dyeing solution to the accessory piece in the step (5) is 1: 5.
Preferably, step (7) is carried out in an oven.
The invention has the beneficial effects that:
the invention changes the water bleaching process of the radix aconiti carmichaeli after being boiled in the traditional processing process into cold soaking to room temperature, which can reduce the loss of effective components and save the processing time.
The invention improves the processing technology of the black cis-trans tablets before and after water bleaching and the processing technological parameters of the black cis-trans tablets, so that the water-soluble extract, the monoester alkaloid content, the diester alkaloid content and the like of the black cis-trans tablets obtained by processing are higher than those of the prior art.
The invention aims at the problem that the processes of removing the gallbladder, decocting, rinsing and the like in the processing process of the existing HEISHUN tablet are not standard; key control parameters lack for key factors such as cooking, steaming, drying time and the like; time and labor are wasted, the yield is low, the reproducibility is poor and the like, and the processing method of the black shun tablets is provided. The method of the invention changes the water bleaching after boiling in Chinese pharmacopoeia into cold soaking to room temperature by optimizing the processing technology; the processing technological parameters of the black tablets are definite, the processing technological process is standardized, and the existing quality standard evaluation is perfected. Compared with the traditional process, the method has the advantages of time saving, labor saving, standardization and better application prospect.
Drawings
FIG. 1 is a graph showing the comparison of mold appearance in low Chouba concentration preservation, where a is 10% Chouba concentration and b is 20% Chouba concentration in Chouba solution after soaking in water at about 30 deg.C for 7 days.
FIG. 2 is a comparison of the processing degree of Fu Zi at different boiling time.
FIG. 3 is a comparison of the effect of different ratios of staining solutions on the appearance of monkshood.
Detailed Description
The invention is described in detail below with reference to the figures and the detailed description of the embodiments.
Example 1 appearance Scoring criteria
The appearance of Chinese medicine is an important evaluation index for the quality of Chinese medicine. According to the character description under the monkshood item of the 'Chinese pharmacopoeia' 2020 edition, 3 indexes of color, texture and taste are selected as investigation objects, and the evaluation standard of the appearance character of the black shun tablets is shown in a table 1:
TABLE 1 Scoring standards for the appearance of Heishin tablets
Figure BDA0003554844750000041
EXAMPLE 2 determination of extract and six ester alkaloids content
Measuring water soluble extract by hot dipping method in extract measuring method (general rule 2201) of 'Chinese pharmacopoeia' 2020 edition; the content of the black matrix is measured according to the content measurement and inspection method of the black matrix in the 2020 version of Chinese pharmacopoeia.
Example 3 comparison of Black flakes quality for optimized Water bleaching Process
According to pharmacopoeia standards, processing specifications of provinces and cities and field investigation conditions, the water bleaching process is usually operated as bleaching overnight. Cleaning the above materials, soaking in aqueous solution of bile for several days, boiling together with the soaking solution until the materials are thoroughly soaked, taking out, rinsing with water, longitudinally cutting into pieces with thickness of about 0.5cm, rinsing with water, dyeing the pieces into dark brown with color matching solution, taking out, steaming to obtain oil surface and luster, drying to semi-dry, and sun-drying or further drying to obtain black smooth pieces 1; cleaning radix Aconiti lateralis Preparata according to size, soaking in aqueous solution of radix Gentianae for several days, decocting together with the extractive solution until it is transparent, taking out, cold soaking to room temperature, longitudinally cutting into slices with thickness of about 0.5cm, soaking and bleaching with water, dyeing the slices with color-adjusting solution to dark brown, taking out, steaming to oil surface and luster, oven drying to semi-dry, and sun drying or oven drying to obtain black tablet 2. Appearance properties, water-soluble extract, monoester alkaloid content, and diester alkaloid content of the Heishi 1 and Heishi 2 were compared. The results are shown in Table 2:
TABLE 2 comparison of the quality of two black flakes
Figure BDA0003554844750000042
The content of monoester alkaloid and diester alkaloid in the optimized water bleaching process is higher than that before optimization, and the content requirements under the item of monkshood in 2020 edition of Chinese pharmacopoeia are met; the time of cold soaking to room temperature can be shortened by about one fourth compared with the time of water rinsing, thereby saving more production time.
Example 4 Single factor investigation of the processing technology of Heishun tablet
And selecting the optimized water bleaching process, and performing single factor investigation on the processing process of the HEISHUN tablets.
1, a bladder making process:
cleaning radix Aconiti lateralis Preparata of Sichuan river oil, removing fibrous root impurities, weighing about 3kg of radix Aconiti lateralis, and placing into stainless steel barrels with gallbladder concentration of 10%, 20%, 30%, and 40% (g/mL). And (3) inspecting the antiseptic effect of the aconitum carmichaeli soaked in different choline concentrations for 10 days, 15 days, 20 days, 25 days and 30 days and the influence degree of the soaked aconitum carmichaeli on the content of the monoester-diester alkaloid.
1.1 anticorrosion effect:
the preservative effect of the low concentration bile bar solution is shown in figure 1.
1.2 the content of ester alkaloids is shown in table 3:
TABLE 3 examination of the content of ester alkaloids
Figure BDA0003554844750000051
2 boiling process
Soaking radix Aconiti lateralis in 30% bile solution for 20 days, taking out, adding about 500g radix Aconiti lateralis into a steamer, adding bile solution in which radix Aconiti lateralis is submerged, decocting for 5min, 10min, 15min and 20min, respectively, and observing the boiling time according to the property of radix Aconiti lateralis decoction and the content of monoester alkaloid.
2.1 degree of concoction
The "full core" state of radix Aconiti lateralis Preparata in different processing (decocting) times is shown in FIG. 2.
2.2 the ester alkaloid content is shown in Table 4:
TABLE 4 monoester alkaloid content
Cooking time (min) Content of monoester type alkaloid (%)
0 0.0064
5 0.0130
10 0.0181
15 0.0136
20 0.0153
3 cutting process
Longitudinally cutting radix Aconiti lateralis into pieces with thickness of about 0.5cm according to "Chinese pharmacopoeia" 2020 edition.
4 water bleaching process
The cut aconite pieces are put into a water tank, because after being soaked and boiled in the bile bar water, the residual bile bar needs to be rinsed with water to reduce the influence of the bile bar water on the quality of the black strips. Therefore, the optimal soaking and bleaching process is determined by performing single factor investigation on the water changing times (1 time/day, 2 times/day, 3 times/day, 4 times/day and 5 times/day) and the water changing days (1, 2 and 3), adding clear water for soaking (1.5 kg of clear water is used for each 1kg of accessory piece) until the water is changed from dirty yellow to milky white and when a large amount of foam is generated, the accessory piece is changed from yellow to white and has no spicy feeling when tasting mouth, and taking the ash content and the acid-insoluble ash content under the monkshood item of 2020 edition of Chinese pharmacopoeia as indexes. Selecting a parameter range in which the content of calcium chloride tends to be stable according to the content change of the calcium chloride in the rinsing liquid; the ash content of the aconite under the item of the Chinese pharmacopoeia 2020 edition is not more than 6.0 percent, the content of the acid insoluble ash content is not more than 1.0 percent as indexes, on the basis of meeting the requirements of the pharmacopoeia, the rinsing days for saving production are selected, and the parameter range of rinsing for 3-5 times within 24h is determined.
4.1 calcium chloride content is shown in Table 5:
TABLE 5 calcium chloride content
Figure BDA0003554844750000061
Figure BDA0003554844750000071
4.2 Ash and acid insoluble Ash content is shown in Table 6:
TABLE 6 determination of Ash and acid insoluble Ash
Figure BDA0003554844750000072
5 dyeing process
The color matching liquid is prepared from sugar, rape oil and water, so that the bleached decoction pieces are dyed into dark brown, the proportion of the sugar, the rape oil and the water is inspected by taking the appearance and the properties in combination with the actual production and the determination of the drug content as indexes, and the optimal color matching process is achieved. The appearance of the dyed aconite piece is observed, so that the type and the mass ratio of the sugar in the dyeing solution are determined to be 1:1:0.5, namely, the ratio of brown sugar to water to rape oil (mass ratio), in consideration of the cost in actual production, and the appearance of the dyed aconite piece meets the requirement of 'dark brown'.
The dyeing effect of the dyeing liquid with different types and proportions is shown in figure 3.
6 steaming process
Putting the dyed accessory piece into a steamer, timing from the round atmosphere, setting horizontal factors for steaming for 2h, 3h, 4h and 5h, wherein the alkaloid content of the accessory piece can change in the heating process, and carrying out process investigation on the steaming time by combining the appearance properties (oily surface and luster) of the accessory piece, the taste without tongue numbness, the diester-type alkaloid limit under the monkshood item in the 2020 edition of Chinese pharmacopoeia and the content measurement of pharmacopoeia. The results are shown in Table 7:
TABLE 7 examination of the steaming Process
Steaming time (h) Content of monoester type alkaloid (%) Diester type alkaloid content (%)
2 0.0117 <0.020
3 0.012 <0.020
4 0.0114 <0.020
5 0.0109 <0.020
7 drying process
Taking out monkshood which is soaked in 30% choline solution for 20 days, boiling the monkshood together with the immersion liquid for 10min, taking out the monkshood, soaking the monkshood in water to room temperature, cutting into pieces with the thickness of about 0.5cm, putting the pieces into the water for rinsing, changing the water for 4 times within 24h, putting the pieces into a steamer for steaming for 3h, taking 5 parts of pieces with the weight of about 500g, and drying the pieces in an electric drum air drying box with the temperature set to be 55 ℃, 60 ℃, 65 ℃, 70 ℃ and 75 ℃ respectively. The contents of single moisture, ester alkaloid and diester alkaloid are taken as indexes, and different drying temperatures are investigated by combining energy consumption. The results are shown in Table 8:
TABLE 8 examination of the drying Process
Drying temperature (. degree.C.) Drying time (h) Water content% Content of monoester alkaloid% Content of monoester alkaloid%
55 9 12.3 0.0294 <0.020
60 7.5 13.9 0.0441 <0.020
65 6 13.3 0.0279 <0.020
70 5.5 12.6 0.0349 <0.020
75 5 10.1 0.0371 <0.020
Example 5 determination of optimum Process by orthogonal experiments
1. Based on the single-factor investigation of the processing process of black tablets under the item of monkshood in 2020 edition of Chinese pharmacopoeia and L 9 (3 4 ) Orthogonal design, test preparation samples are arranged according to an orthogonal table. Appearance, water-soluble extract, monoester typeThe processing method of HEISHUI tablet is preferred, and the alkaloid content and diester alkaloid content are used as indexes. The levels of the factors are shown in Table 9, and the results and analysis are shown in tables 10 and 11.
TABLE 9 HORIZONTAL DESIGN FACTOR LEVEL METER FOR BLACK-AND-SHRIGHT-SHEET
Figure BDA0003554844750000081
TABLE 10 orthogonal test results of the processing technique of Heishun tablets
Figure BDA0003554844750000082
Figure BDA0003554844750000091
TABLE 11 orthogonal experimental visual analysis of the processing technique of Heishun tablet
Figure BDA0003554844750000092
2. And (3) carrying out variance analysis on the orthogonal test results:
2.1 analysis of variance: appearance character
Figure BDA0003554844750000101
F 0.05(2,2) =19.00,F 0.01(2,2) =9
2.2 analysis of variance: content of extract%
Figure BDA0003554844750000102
F 0.05(2,2) =19.00,F 0.01(2,2) =9
2.3 analysis of variance: content of monoester alkaloid%
Figure BDA0003554844750000103
F 0.05(2,2) =19.00,F 0.01(2,2) =9
2.4 analysis of variance: content of diester-type alkaloids%
Figure BDA0003554844750000104
F 0.05(2,2) =19.00,F 0.01(2,2) =9
Through analysis of orthogonal test results, the influence of the drying temperature on appearance properties is remarkably different, and the influence of boiling time, water bleaching times and steaming time on the content of the monoester alkaloid is remarkably different. According to the processing process flow and the examination and content measurement items of the black shun tablets under the item of monkshood in the 'Chinese pharmacopoeia' 2020 edition, the optimal processing process of the black shun tablets is determined as follows: cleaning radix Aconiti lateralis Preparata, soaking in 30% aqueous solution of bile for 20 days, decocting together with the soaking solution for 10min, taking out, soaking and bleaching to room temperature, longitudinally cutting into pieces with thickness of about 0.5cm, bleaching with water for 4 times within 24h, dyeing the pieces into dark brown with a color mixing solution containing brown sugar, water and rape oil (mass ratio) of 1:1:0.5, taking out, steaming for 3h, oven drying at 65 deg.C for 6h, and taking out.
Example 6 best process verification
Cleaning radix Aconiti lateralis Preparata according to size, soaking in 30% aqueous solution of choline (choline chloride) for 20 days, decocting together with the extractive solution for 10min, taking out, leaching to room temperature, longitudinally cutting into pieces with thickness of 0.5cm, rinsing with water for 4 times within 24h, dyeing the pieces into dark brown with brown sugar, water and vegetable oil (mass ratio) of 1:1:0.5, taking out, steaming for 3h, oven drying at 65 deg.C for 6h, and taking out. 3 samples are prepared in parallel by the process, and the RSD values of extracts and black strips of the 3 parallel samples prepared by the optimal process are less than 3.0 percent, which indicates that the process is reasonable and feasible, and the results are shown in a table 11.
TABLE 12 verification of the best processing procedure
Figure BDA0003554844750000111
The invention optimizes the processing technology of the black shun slice decoction pieces and determines the processing technological parameters of the black shun slice decoction pieces in 'Chinese pharmacopoeia' of 2020 edition. The processing technology is stable and feasible, the production efficiency is improved compared with the technology before optimization, and the parameters are clear. Provides important basis for establishing quality control of high-quality black shun tablet, saves time and labor, has the advantages of standardization and good application prospect.

Claims (10)

1. A processing method of Heishun tablet is characterized by comprising the following steps:
cleaning radix Aconiti lateralis Preparata, soaking gallbladder, decocting, slicing, rinsing with water, dyeing, steaming in water, and drying;
wherein, the process parameters are determined by the following method:
taking the appearance, the content of water-soluble extract, monoester alkaloid and diester alkaloid as evaluation indexes, carrying out single-factor investigation by taking the concentration of bile, the time for soaking bile, the boiling time, the number of times of water bleaching, the proportion of dyeing liquid, the steaming time and the drying temperature as variables, determining the concentration of bile, the time for soaking bile and the proportion of dyeing liquid, determining the parameter ranges of the boiling time, the number of times of water bleaching, the steaming time and the drying temperature, and designing an orthogonal test;
obtaining an experimental result of an orthogonal test, determining the influence degree of each factor by combining the visual analysis of the orthogonal test and the variance analysis, determining the optimal process parameters, and processing the black strips by using the determined optimal process parameters.
2. The processing method according to claim 1, wherein the evaluation method of the appearance properties is: and (4) scoring the black strips from the aspects of color, texture and mouthfeel, and taking the total score as an index value of the appearance character.
3. The processing method according to claim 1, wherein the concentration of the bile and the time for bile infusion are determined by: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, then respectively putting the monkshood into the gallbladder solutions with different concentrations, observing the antiseptic effect of the solutions, obtaining the contents of the monoester alkaloid and the diester alkaloid after gallbladder soaking, taking the gallbladder solution without mould in 30 days as a premise, selecting the gallbladder soaking time which is appropriate and corresponds to the time when the ratio of the contents of the monoester alkaloid and the diester alkaloid is maximum as an intermediate time, and determining the gallbladder concentration and the gallbladder soaking time.
4. The processing method of claim 1, wherein the parameter range of the boiling time is determined by: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of bile and the time for soaking bile, boiling in a bile solution for different times, observing the central character of monkshood and obtaining the content of monoester alkaloid, selecting the boiling time which reaches the throughout standard specified in Chinese pharmacopoeia and has the highest content of monoester alkaloid as the intermediate time, and determining the parameter range of the boiling time.
5. The processing method according to claim 1, wherein the parameter range of the number of water drifts is determined by: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of gallbladder, the gallbladder soaking time and the boiling time, respectively soaking in clean water after slicing, changing water for a soak solution at a fixed frequency in the soaking process, investigating the content of calcium chloride and the content of ash and acid-insoluble ash in the soak solution during each water change, selecting a soak solution with the ash content and the acid-insoluble ash content lower than the limit of the ash content and the acid-insoluble ash content specified in Chinese pharmacopoeia, and selecting a water bleaching frequency range with proper water bleaching frequency and stable calcium chloride content.
6. The processing method according to claim 1, wherein the ratio of the dyeing liquid is determined by: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of bile, the bile soaking time and the boiling time, respectively adding clear water to soak after slicing, fixing the water changing times in the soaking process, soaking in different dyeing solutions for dyeing, observing the appearance color of the dyed monkshood, and determining the proportion of the dyeing solutions based on the dark brown.
7. The processing method of claim 1, wherein the parameter range of the steaming time is determined in a manner that: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of bile, the bile soaking time and the boiling time, respectively adding clear water for soaking after slicing, fixing the water changing times in the soaking process, then soaking in dyeing solution with the same components for dyeing, then respectively steaming, timing from round air, steaming for different times, observing the appearance of steamed monkshood and obtaining the content of monoester alkaloid and the content of diester alkaloid, selecting the steaming time which is lower than the limit of diester alkaloid specified in Chinese pharmacopoeia and has the highest content of monoester alkaloid as the middle time, and determining the parameter range of the steaming time.
8. The processing method according to claim 1, wherein the parameter range of the drying temperature is determined by: taking a plurality of groups of cleaned monkshood to remove fibrous root impurities, fixing the concentration of bile, the bile soaking time and the boiling time, respectively adding clear water to soak after slicing, fixing the water changing times in the soaking process, soaking in dyeing solution with the same components for dyeing, fixing the steaming time, then drying at different temperatures to obtain the content of monoester alkaloid and the content of diester alkaloid, selecting drying with the diester alkaloid content lower than the limit specified in Chinese pharmacopoeia and the highest monoester alkaloid content as intermediate time, and determining the parameter range of drying.
9. The processing method of the Heishun tablet is characterized by comprising the following steps:
(1) and (3) soaking the liner: soaking the cleaned monkshood in a choline solution for 20 days, wherein the concentration of the choline solution is 30% (g/mL);
(2) boiling: decocting the soaked radix Aconiti lateralis and the gallbladder solution for 10min, and soaking to room temperature;
(3) slicing: slicing the monkshood obtained in the step (2) to obtain monkshood slices;
(4) rinsing with water: carrying out water rinsing on the monkshood slices, wherein water is changed for 4 times within 24 hours in the water rinsing process;
(5) dyeing: dyeing the water-bleached monkshood slices with a dyeing solution; in the dyeing liquid, the mass ratio of brown sugar, water and rape oil is 1:1: 0.5;
(6) steaming: steaming the dyed radix Aconiti lateralis in a container for 3h after air circulation;
(7) and (3) drying: the steamed monkshood slices are dried for 6h at 65 ℃.
10. The processing method according to claim 9, wherein the cleaning in step (1) is to clean the rhizoma typhonii respectively according to size;
the slicing in the step (3) is performed by adopting a slicing machine;
the slice in the step (3) is cut to 0.5cm in thickness;
in the step (5), the mass ratio of the dyeing liquid to the accessory pieces is 1: 5;
and (7) performing in an oven.
CN202210273064.3A 2022-03-19 2022-03-19 Processing method of Heishun tablet Pending CN114917276A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116637139A (en) * 2023-06-26 2023-08-25 城固县群利中药材专业合作社 Dry accessory slices for fixation and preparation method thereof, black accessory slices and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116637139A (en) * 2023-06-26 2023-08-25 城固县群利中药材专业合作社 Dry accessory slices for fixation and preparation method thereof, black accessory slices and preparation method thereof

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