CN116966231A - Method for processing radix scrophulariae in fresh place - Google Patents

Method for processing radix scrophulariae in fresh place Download PDF

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Publication number
CN116966231A
CN116966231A CN202310993227.XA CN202310993227A CN116966231A CN 116966231 A CN116966231 A CN 116966231A CN 202310993227 A CN202310993227 A CN 202310993227A CN 116966231 A CN116966231 A CN 116966231A
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radix scrophulariae
processing
fresh
drying
namely
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Inventor
张哲雯
杜伟锋
杨柳
康显杰
李小宁
叶佩
章龙
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ZHEJIANG CHINESE MEDICAL UNIVERSITY MEDICAL PIECES CO LTD
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ZHEJIANG CHINESE MEDICAL UNIVERSITY MEDICAL PIECES 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)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/80Scrophulariaceae (Figwort family)
    • A61K36/808Scrophularia (figwort)
    • 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/13Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
    • 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • 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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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to the technical field of radix scrophulariae processing, in particular to a method for processing radix scrophulariae in a fresh place, which comprises the following steps: s1: cleaning, namely, preparing fresh radix scrophulariae, removing impurities, and cleaning with clear water; s2: sweating, semi-drying, spreading the cleaned radix scrophulariae for 5 to 7 days, and piling up the radix scrophulariae for sweating for 2 days after the radix scrophulariae is dried in the semi-drying state; s3: cutting, namely slicing the obtained radix scrophulariae; s4: drying, namely spreading and airing the thin radix scrophulariae overnight, and drying the radix scrophulariae by using an oven; s5: sieving, sieving with XSR-3B flexible support inclined plane sieving machine to remove ash and dust to obtain radix scrophulariae decoction pieces; s6: quality inspection is carried out according to the Chinese pharmacopoeia of 2020 edition, and the quality inspection is compared with the traditional processed decoction pieces. The invention simplifies the processing flow of radix scrophulariae, avoids repeated operation of the process, avoids secondary loss of active ingredients, and ensures the quality of radix scrophulariae medicinal materials.

Description

Method for processing radix scrophulariae in fresh place
Technical Field
The invention relates to the technical field of radix scrophulariae processing, in particular to a method for processing radix scrophulariae in a fresh place.
Background
The processing of the traditional Chinese medicine production place is an important link of the production of the traditional Chinese medicine. The newly harvested Chinese medicinal materials generally need to be subjected to primary processing at the production place. The primary processing aims are mainly as follows: removing non-medicinal parts and impurities, separating different medicinal parts, changing medicinal materials, killing enzyme and protecting glycoside, reducing or eliminating toxicity or side effects of the medicine, etc. The traditional Chinese medicine processed by the producing area generally meets the requirements of complete shape, moderate water content, good color, little fragrance loss, no change of taste, little destruction or loss of active ingredients and the like.
The fresh radix scrophulariae is picked up in winter when stems and leaves wilt, rhizome, bud, fibrous root and silt are removed, sun-dried or baked to be semi-dry, piled up for 3-6 days, and repeatedly dried for several times to form the radix scrophulariae. After reaching the decoction piece enterprise, carrying out secondary processing, namely taking the raw materials, removing residual rootstocks and impurities, cleaning, moistening thoroughly, slicing and drying; or soaking in micro-bubble, steaming, cooling, slicing, and drying to obtain radix scrophulariae decoction pieces. The prior art can cause the cross repetition of the production process of the production place processing and the processing of the decoction piece factory, the complex processing procedures and the secondary loss of the medicinal components. Not only wasting labor cost and resource cost, but also affecting the quality of the traditional Chinese medicine decoction pieces, and being easy to cause unqualified quality of the decoction pieces, especially the content of the water-soluble extract of the figwort root and the content of the important water-soluble components harpagoside and harpagoside. In order to standardize the processing of the traditional Chinese medicine material in the production place, so as to achieve the purposes of optimizing production links, facilitating storage and transportation, reducing cost, improving quality of decoction pieces and the like, the traditional Chinese medicine material is suggested to be processed while the production place is fresh, namely the traditional Chinese medicine material is cut into pieces at the production place and then dried. According to the characteristic that radix scrophulariae needs to sweat and dry, semi-fresh processing keeping traditional characteristics is selected: the fresh medicinal materials are firstly subjected to sweating processing according to the traditional method in the production place, and the medicinal materials are directly sliced after being dried to a certain degree. Therefore, how to simplify the processing procedures of the producing area processing and the processing, remove repeated procedures and improve the quality of decoction pieces as much as possible is a problem to be solved at present.
Disclosure of Invention
The invention aims to provide a method for processing radix scrophulariae in a fresh place, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for processing radix scrophulariae in a fresh place comprises the following steps:
s1: cleaning, namely, preparing fresh radix scrophulariae, removing impurities, and cleaning with clear water;
s2: sweating, semi-drying, spreading the cleaned radix scrophulariae for 5 to 7 days, and piling up the radix scrophulariae for sweating for 2 days after the radix scrophulariae is dried in the semi-drying state;
s3: cutting, namely slicing the obtained radix scrophulariae;
s4: drying, namely spreading and airing the thin radix scrophulariae overnight, and drying the radix scrophulariae by using an oven;
s5: sieving, sieving with XSR-3B flexible support inclined plane sieving machine to remove ash and dust to obtain radix scrophulariae decoction pieces;
s6: quality inspection is carried out according to the Chinese pharmacopoeia of 2020 edition, and the quality inspection is compared with the traditional processing.
Preferably, a roller medicine washing machine is used for washing radix scrophulariae, and the washing time is not less than 30 minutes.
Preferably, the step S2 is repeated 2 to 3 times.
Preferably, the radix scrophulariae is cut by using a QYJ-300 type linear reciprocating slicer, and the slicing thickness is 1-2 mm.
Preferably, the radix scrophulariae slices are dried by adopting an RXH-27-C type oven, and the baking time is not less than 6 hours at the temperature of 75 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention simplifies the processing flow of radix scrophulariae, avoids repeated operation of the process, avoids secondary loss of active ingredients, and ensures the quality of radix scrophulariae medicinal materials.
Drawings
FIG. 1 is a flow chart of a conventional radix scrophulariae processing process;
FIG. 2 is a flow chart of a fresh radix scrophulariae processing technology in the invention;
FIG. 3 is a diagram of four batches of crude drug samples;
FIG. 4 is a diagram of a conventional processed radix scrophulariae decoction piece;
FIG. 5 is a diagram of a radix scrophulariae decoction piece processed while fresh;
FIG. 6 is a microscopic identification chart;
FIG. 7 is a thin layer diagram of a traditional processed decoction piece of radix scrophulariae and a processed decoction piece while fresh;
FIG. 8 is a chromatogram of a standard;
FIG. 9 is a chromatogram of a freshly processed sample;
FIG. 10 is a chromatogram of a conventional processed sample.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1 to 10, the present invention provides a technical solution: a method for processing radix scrophulariae in a fresh place comprises the following steps:
s1: cleaning, namely, preparing fresh radix scrophulariae, removing impurities, and cleaning with clear water;
s2: sweating, semi-drying, spreading the cleaned radix scrophulariae for 5 to 7 days, and piling up the radix scrophulariae for sweating for 2 days after the radix scrophulariae is dried in the semi-drying state;
s3: cutting, namely slicing the obtained radix scrophulariae;
s4: drying, namely spreading and airing the thin radix scrophulariae overnight, and drying the radix scrophulariae by using an oven;
s5: sieving, sieving with XSR-3B flexible support inclined plane sieving machine to remove ash and dust to obtain radix scrophulariae decoction pieces;
s6: quality inspection is carried out according to the Chinese pharmacopoeia of 2020 edition, and the quality inspection is compared with the traditional processing.
When the radix scrophulariae is cleaned, a roller medicine cleaning machine is used, and the cleaning time is not less than 30 minutes.
The step S2 is repeated for 2 to 3 times.
The radix scrophulariae is cut by using a QYJ-300 type linear reciprocating slicer with the slicing thickness of 1-2 mm.
When the figwort slices are dried, an RXH-27-C type oven is adopted, and the baking time is not less than 6 hours at the temperature of 75 ℃.
The invention simplifies the processing flow of radix scrophulariae, avoids repeated operation of the process, avoids secondary loss of active ingredients, and ensures the quality of radix scrophulariae medicinal materials; the preparation method is mainly suitable for the preparation process of fresh radix scrophulariae production area, and ensures the quality of radix scrophulariae, wherein the grasping of parameters such as sweating time and sweating frequency is key.
Collecting 4 batches of raw medicinal materials, and processing according to the traditional processing technology and the fresh processing technology respectively to prepare traditional processing tablets at the production place and fresh processing tablets. The information of the medicinal material samples is shown in the following table.
Radix scrophulariae medicinal material sample information
The traditional method is adopted to process the raw materials, four batches of raw materials are respectively taken for processing, the detailed technological parameters are shown in the following table,
detailed technological parameters for traditional processing of radix scrophulariae decoction pieces
The obtained decoction pieces are shown in FIG. 4.
The four batches of crude drugs are processed in a fresh processing mode, the details of the processing technology are shown in the following table,
detailed technological parameters for processing radix scrophulariae decoction pieces while fresh
The obtained decoction piece picture is shown in figure 5.
The two processing modes of decoction pieces have certain differences in properties, and the traditional processing pieces are as follows: the product is round or elliptic sheet. The outer epidermis is yellowish or brownish. The section is black, slightly glossy and has cracks. The qi is peculiar like caramel, sweet and slightly bitter.
Processing the slices while fresh: the product is round or elliptic sheet. The outer epidermis is yellowish or brownish and the epidermis is slightly wrinkled. Black section, slightly glossy; or black brown, unsmooth surface, and some cracks. The qi is peculiar like caramel, sweet and slightly bitter.
Microscopic identification: the product has a cross section: the cortex is wider, stone cells are scattered singly or 2-5 are clustered, polygonal, round-like or square-like, the wall is thicker, and the layering is obvious. Phloem rays are multi-slit. Forming a layer into a ring. The xylem has wide rays and multiple cracks; the few ducts, polygonal-like, have diameters of about to 113 μm, with wood fibers. Parenchyma cells contain nuclei.
Thin layer authentication: taking 2g of the product powder, adding 25mL of methanol, soaking for 1 hour, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 25mL of water into the residue to dissolve, carrying out shaking extraction for 2 times with water saturated n-butanol for 30mL each time, combining n-butanol solutions, evaporating to dryness, and adding 5mL of methanol into the residue to dissolve, thereby obtaining a sample solution. 2g of radix scrophulariae is prepared as a control medicinal material, and the control medicinal material solution is prepared by the same method. And adding methanol into the harpagoside reference substance to prepare a solution with 1mg per 1mL serving as a reference substance solution. According to a thin layer chromatography (general rule 0502) test, sucking 4 mu L of each of the three solutions, respectively spotting on the same silica gel G thin layer plate, taking the lower layer solution of chloroform-methanol-water (12:4:1) as a developing agent, placing into a developing cylinder presaturated for 15 minutes with the developing agent, developing, taking out, airing, spraying 5% vanillin sulfuric acid solution, and blowing hot air until the spots develop clearly. In the sample chromatogram, spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram. In FIG. 7, S is harpagoside and harpagoside standard, M is control medicinal material, CT1-4 is traditional decoction piece, CX1-4 is fresh decoction piece.
The decoction pieces of two different batches were checked for moisture, total ash and acid insoluble ash. When checking moisture, 2-5 g of the test sample is taken and spread in a flat weighing bottle which is dried to constant weight, the thickness is not more than 5mm, the loose test sample is not more than 10mm, the precision weighing is carried out, a bottle cover is opened, the bottle cover is dried for 5 hours at 100-105 ℃, the bottle cover is covered, the bottle cover is moved into a dryer, the bottle cover is cooled for 30 minutes, the precision weighing is carried out, the bottle cover is dried for 1 hour at the temperature, the bottle cover is cooled and the bottle cover is weighed until the difference between two continuous weighing is not more than 5 mg. The water content (%) in the test sample was calculated based on the weight loss. When checking total ash, the test sample for measurement needs to be crushed, and the test sample can pass through a second sieve, and after being uniformly mixed, 2 to 3g of the test sample is taken and placed into a crucible with constant weight to be burnt, the weight is weighed, the combustion is avoided by slow heating, and when the test sample is completely carbonized, the temperature is gradually increased to 500 to 600 ℃ to ensure that the test sample is completely ashed and reaches the constant weight. The total ash content (%) in the test sample was calculated from the weight of the residue. When the acid insoluble ash was examined, the ash obtained in the total ash item was taken, diluted hydrochloric acid was carefully added to about 10mL in the crucible, the crucible was covered with a petri dish, the residue in the crucible was washed with water on paper, and washed until no chloride reaction was observed in the washing liquid. The filter residue together with the filter paper is transferred to the same crucible, dried and burned to constant weight. The content (%) of acid-insoluble ash in the sample was calculated from the weight of the residue. As shown in the table below.
Comparison table of traditional processing and fresh processing of radix scrophulariae decoction pieces for moisture, total ash and acid insoluble ash
Conclusion: the water content, ash content and acid insoluble ash content of the radix scrophulariae decoction pieces processed in the traditional way and the fresh way all meet pharmacopoeia standards.
The samples were subjected to extract detection as determined by hot dip methods under the water-soluble extract assay (general rule 2201).
About 2-4 g of the sample is taken, precisely weighed, placed in a conical flask with 100-250 mL, precisely added with 50-100 mL of water, sealed, weighed, kept stand for 1 hour, connected with a reflux condenser tube, heated to boiling, and kept slightly boiling for 1 hour. After cooling, the conical flask is taken down, the sealing is carried out, the weight is weighed again, the lost weight is complemented by water, the shaking is carried out, the filtering is carried out by a drying filter, 25mL of filtrate is precisely measured, the filtrate is placed in an evaporation dish which is dried to constant weight, the evaporation dish is dried by evaporation on a water bath, the drying is carried out for 3 hours at 105 ℃, the cooling is carried out for 30 minutes in a dryer, and the weight is rapidly and precisely weighed. The content (%) of the water-soluble extract in the test sample was calculated on the basis of the dried product, unless otherwise specified, and the details are shown in the following table.
Comparison table of traditional processing and fresh processing extracts of radix scrophulariae decoction pieces
Conclusion: the extract item, the traditional processing and the fresh processing of the figwort decoction pieces meet the pharmacopoeia standard. The extract yield is obviously higher than the pharmacopoeia standard in the traditional processing and the fresh processing of the figwort decoction pieces, the fresh processing of the figwort decoction pieces is slightly higher than the traditional processing of the figwort decoction pieces, the average value of the traditional processing group is 74.05%, the standard deviation is 0.0458, the average value of the fresh processing group is 80.46%, and the standard deviation is 0.0383. P=0.810, P > 0.05, the overall variance of the two groups can be considered to be irregular, t=1.433, double-sided p=0.076 > 0.05, the difference between the two groups is not significant, and the traditional processing group can be considered to be equivalent to the processing group when it is fresh.
Content measurement, according to high performance liquid chromatography (general rule 0512). Chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; acetonitrile is taken as a mobile phase A, 0.03% phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specifications in the following table; the detection wavelength is 210nm, and the theoretical plate number is not less than 5000 according to the harpagoside and harpagoside peaks.
Gradient elution meter
Preparation of a control solution: taking a proper amount of harpagoside reference substance and harpagoside reference substance, precisely weighing, and adding 30% methanol to prepare a mixed solution containing 60 mug of harpagoside and 20 mug of harpagoside per 1 mL.
Preparation of test solution: taking about 0.5g of the powder (sieving with a third sieve), precisely weighing, placing into a conical flask with a plug, precisely adding 50mL of 50% methanol, sealing, weighing, soaking for 1 hour, performing ultrasonic treatment (power 500W, frequency 40 kHz) for 45 minutes, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking uniformly, filtering, and taking subsequent filtrate.
Assay: respectively precisely sucking 10 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The chromatogram of the standard product is shown in fig. 8, and the chromatograms of the fresh processed sample and the traditional processed sample are shown in fig. 9 and 10, wherein '1' represents harpagoside and '2' represents harpagoside. Data from the chromatograms are detailed in the following table.
Comparison table for measuring content of radix scrophulariae decoction pieces in traditional processing and fresh processing
From the content measurement results, the contents of the traditional processing sample and the fresh processing sample both accord with the pharmacopoeia standard and are obviously higher than that of the pharmacopoeia, the harpagoside component is higher than that of the traditional processing sample in the aspect of Anhui and Sichuan, and the contents of the Hubei and Chongqing are lower than that of the traditional processing sample in the aspect of fresh processing, which may be related to the fact that the Hubei and Chongqing do not have the process of sweating for many times in the aspect of fresh processing samples. The mean value of the traditional processing group of the harpagoside content is 1.16%, the standard deviation is 0.0029, the mean value of the processing group while fresh is 1.22%, and the standard deviation is 0.0032. P=0.859 > 0.05, the overall variance of the two groups cannot be considered to be uneven, t=0.277, double sided p=0.791 > 0.05, the difference between the two groups of data is not significant, and the traditional processing group can be considered to be equivalent to the processing group when it is fresh.
The mean value of the traditional processing group of harpagoside content is 0.31%, the standard deviation is 0.0003, the mean value of the fresh processing group is 0.39%, and the standard deviation is 0.0022. P=0.117 > 0.05, the overall variance of the two groups cannot be considered to be uneven, t=0.695, double sided p=0.513 > 0.05, the difference between the two groups of data is not significant, and the traditional processing group can be considered to be equivalent to the processing group when it is fresh.
Conclusion: from the average value of extract and content measurement results, the fresh radix scrophulariae is processed better than the traditional processing, but the fresh radix scrophulariae has no significant difference, and the fresh radix scrophulariae is considered to be equivalent to the traditional processing. And the processing process is simple and convenient, so that the fresh processing of the radix scrophulariae in the producing area is supported.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. A method for processing radix scrophulariae in a fresh place is characterized by comprising the following steps: the method comprises the following steps:
s1: cleaning, namely, preparing fresh radix scrophulariae, removing impurities, and cleaning with clear water;
s2: sweating, semi-drying, spreading the cleaned radix scrophulariae for 5 to 7 days, and piling up the radix scrophulariae for sweating for 2 days after the radix scrophulariae is dried in the semi-drying state;
s3: cutting, namely slicing the obtained radix scrophulariae;
s4: drying, namely spreading and airing the thin radix scrophulariae overnight, and drying the radix scrophulariae by using an oven;
s5: sieving, sieving with XSR-3B flexible support inclined plane sieving machine to remove ash and dust to obtain radix scrophulariae decoction pieces;
s6: quality inspection is carried out according to the Chinese pharmacopoeia of 2020 edition, and the quality inspection is compared with the traditional processing.
2. The method for processing radix scrophulariae while fresh according to claim 1, wherein: when the radix scrophulariae is cleaned, a roller medicine cleaning machine is used, and the cleaning time is not less than 30 minutes.
3. The method for processing radix scrophulariae while fresh according to claim 1, wherein: the step S2 is repeated for 2 to 3 times.
4. The method for processing radix scrophulariae while fresh according to claim 1, wherein: the radix scrophulariae is cut by using a QYJ-300 type linear reciprocating slicer with the slicing thickness of 1-2 mm.
5. The method for processing radix scrophulariae while fresh according to claim 1, wherein: when the figwort slices are dried, an RXH-27-C type oven is adopted, and the baking time is not less than 6 hours at the temperature of 75 ℃.
CN202310993227.XA 2023-08-08 2023-08-08 Method for processing radix scrophulariae in fresh place Pending CN116966231A (en)

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