CN116832124A - Method for preparing glabrous greenbrier rhizome extract - Google Patents
Method for preparing glabrous greenbrier rhizome extract Download PDFInfo
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- CN116832124A CN116832124A CN202310162697.1A CN202310162697A CN116832124A CN 116832124 A CN116832124 A CN 116832124A CN 202310162697 A CN202310162697 A CN 202310162697A CN 116832124 A CN116832124 A CN 116832124A
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/90—Smilacaceae (Catbrier family), e.g. greenbrier or sarsaparilla
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
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- Medical Informatics (AREA)
- Botany (AREA)
- Biotechnology (AREA)
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Abstract
The invention relates to the technical field of smilax glabra extraction, in particular to a method for preparing smilax glabra extract. The method comprises the steps of soaking glabrous greenbrier rhizome decoction pieces in water, performing water bath leaching at 65-75 ℃ to obtain a liquid medicine, filtering the liquid medicine, adding water for decoction, filtering, concentrating the filtrate, and drying to obtain the rhizoma smilacis glabrae decoction pieces, wherein the formation of insoluble matters in the extract is obviously reduced, the improvement effect on the solubility is most obvious, and the astilbin content is obviously improved.
Description
Technical Field
The invention relates to the technical field of smilax glabra extraction, in particular to a method for preparing smilax glabra extract.
Background
Rhizoma Smilacis Glabrae is dry rhizome of Smilax glabra Roxb of Liliaceae, has sweet and light taste, and has effects of nourishing liver, stomach, and spleen channels, removing toxic substances, removing dampness, and dredging joint, and can be used for treating limb contracture and arthralgia and myalgia caused by syphilis and mercury poisoning; damp-heat stranguria with turbid urine, leukorrhagia, carbuncle, scrofula, scabies, etc. Rhizoma smilacis glabrae is commonly used for treating hyperuricemia and gout in clinic. Modern researches have shown that rhizoma Smilacis Glabrae has many pharmacological activities such as anti-inflammatory, analgesic, anti-tumor, antioxidant, immunoregulatory, liver protecting, diuretic, and antibacterial.
The glabrous greenbrier rhizome formula granule is prepared by the processes of water extraction, separation, concentration, drying, granulation and the like of glabrous greenbrier rhizome decoction pieces. Compared with the traditional decoction, the decoction has the advantages of convenient preparation, convenient production and use, accurate dosage, portability and addition and subtraction according to symptoms. However, the previous investigation of the subject group finds that a large amount of undissolved particles still exist after a part of commercial glabrous greenbrier rhizome formula particles are added with 200mL of hot water and stirred for 5min (as shown in figure 1), and similar problems exist in all glabrous greenbrier rhizome formula particles of 3 different source manufacturers, which do not meet the quality requirements of granules specified in Chinese pharmacopoeia of 2020 edition.
The presence of large amounts of insolubles can reduce patient acceptance and compliance with the service, resulting in a decrease in the market competitiveness of the product. In order to improve the solubility of glabrous greenbrier rhizome formula particles, the problem group is to improve the solubility by improving auxiliary materials and a production process in the early stage. However, the methods of auxiliary material screening, dispersant addition, powder modification, extraction time shortening, extraction solution centrifugation to remove sediment and the like cannot effectively solve the problem of poor solubility of glabrous greenbrier rhizome formula particles.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect of poor granule solubility of the glabrous greenbrier rhizome extract in the prior art, thereby providing a method for preparing the glabrous greenbrier rhizome extract.
The invention provides a method for preparing glabrous greenbrier rhizome extract, which comprises the steps of soaking glabrous greenbrier rhizome decoction pieces in water, carrying out water bath leaching at 65-75 ℃ to obtain liquid medicine, filtering the liquid medicine, adding water for decoction, filtering, concentrating the filtrate, and drying.
Further, the times of water bath leaching are 1-5 times, and the time of each water bath leaching is 2-4 hours; preferably, the number of times of water bath leaching is 2-3, and the time of each water bath leaching is 2.5-3.5h.
Further, the number of times of water bath leaching is 2, and the time of each water bath leaching is 2 hours.
Further, the temperature of the water bath leaching is 70 ℃.
Further, adding 6-10 times of water for soaking before water bath leaching.
Further, soaking is carried out at room temperature for 20-40min.
Further, the mass of water added in the water adding and decocting process is 5-8 times of the mass of rhizoma smilacis glabrae decoction pieces, and the water adding and decocting time is 2-4 hours.
Further, the ratio of the volume of the concentrated liquid medicine to the mass of the glabrous greenbrier rhizome decoction pieces is 1.5-2L:2kg.
Further, soaking rhizoma Smilacis Glabrae decoction pieces in 8 times of water for 30min, directly leaching in 70deg.C water bath for 2 hr, filtering with 120 mesh sieve, decocting with 6 times of water for 2 hr, pouring out medicinal liquid, filtering with 120 mesh sieve, mixing filtrates, concentrating, and drying.
The invention also provides the glabrous greenbrier rhizome extract prepared by the method for preparing the glabrous greenbrier rhizome extract.
The invention also provides glabrous greenbrier rhizome formula particles, which comprise glabrous greenbrier rhizome extract prepared by any one of the methods for preparing glabrous greenbrier rhizome extract.
The technical scheme of the invention has the following advantages:
the method for preparing the glabrous greenbrier rhizome extract comprises the steps of soaking glabrous greenbrier rhizome decoction pieces in water, carrying out water bath leaching at the temperature of 65-75 ℃ to obtain liquid medicine, filtering the liquid medicine, then adding water for decoction, filtering, concentrating filtrate, and drying to obtain the glabrous greenbrier rhizome extract, wherein the water bath leaching method at the specific temperature after the water soaking is adopted not only remarkably improves the dissolubility of the glabrous greenbrier rhizome extract, but also remarkably improves the astilbin content, remarkably reduces the decomposition speed of flavonoid compounds, improves the total flavone content, especially the optimal water bath leaching temperature is 70 ℃, and the astilbin content obtained by the water bath leaching is the highest, and only adopts water as a solvent, thereby conforming to the national standard of formula particles.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the dissolution of glabrous greenbrier rhizome formula particles of different manufacturers in the background art;
FIG. 2 shows dissolution of rhizoma Smilacis Glabrae extracts prepared in examples and comparative examples;
FIG. 3 is an insoluble matter ratio (%) of the rhizoma Smilacis Glabrae extracts prepared in examples and comparative examples;
FIG. 4 is a graph showing the change in transmitted light of the smilax glabra extract solutions prepared in examples and comparative examples; a is comparative example 1, B is comparative example 2, C is comparative example 3, D is comparative example 4, E is example 1;
FIG. 5 is a TSI change trend graph;
FIG. 6 is a radar chart of the overall TSI value, bottom and top transmitted intensity averages, top and bottom peak thickness averages of the extract solution;
FIG. 7 is a UPLC characteristic map of rhizoma Smilacis Glabrae extract prepared by five extraction methods; peak 1 is astilbin peak; peak 5 is Engelhardtia chrysolepis Hance.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Instrument:
BSA 224SA model ten-thousandth analytical balance and BT25S model ten-thousandth analytical balance (Sartorius company, germany); water bath (Beijing Zhongxing Wei industry instruments Co., ltd.); electrothermal sleeve (Beijing family Yongxing instruments Co., ltd.); deionized water (Sichuan Upoaching technology Co., ltd.); electrothermal constant temperature blast drying oven (Shanghai Kaila instrumentation factory); freeze dryer (Ningbo Xinzhi freeze drying equipment Co., ltd.); ultimate 3000UPLC high performance liquid chromatograph (Thermo Fisher Scientific); turboiscan Lab stability Analyzer (French formula).
Reagent:
rhizoma Smilacis Glabrae control (ID: 61T 3-EPRG) is purchased from China food and drug inspection institute; astilbin (lot number: DST201015-054, purity not less than 98%), engelhardtia (lot number: DST210604-045, purity not less than 98%), D (+) -anhydrous glucose (lot number: DSTW000501, purity not less than 98%) were all purchased from Lemeitian medicine/Desmot organism; starch kit (south Beijing built bioengineering institute); glacial acetic acid (colone chemicals limited of chengdou) is chromatographic purity; acetonitrile (Anhui Tiandi high purity solvent Co., ltd.) and methanol (Sigma Aldrich trade Co., ltd.) were chromatographically pure; the water is ultrapure water and the other reagents are analytically pure. Four batches of rhizoma Smilacis Glabrae decoction pieces were purchased from Guangxi, hunan, guizhou, sichuan respectively, and identified as dried rhizome of Smilax glabra Roxb.
Example 1
The embodiment provides a preparation method of a glabrous greenbrier rhizome extract, which comprises the following steps:
s1, step: taking 2kg of glabrous greenbrier rhizome decoction pieces, adding 8 times of water, soaking for 30min;
s2, step: directly leaching for 2 times at 70 ℃ in water bath temperature for 2 hours each time to obtain liquid medicine;
s3, step: pouring out the liquid medicine, filtering with 120 mesh sieve, decocting with 6 times of water for 2 hr, pouring out the liquid medicine, and filtering with 120 mesh sieve. Mixing filtrates, concentrating to 1.8L, and drying to obtain powder.
Comparative example 1
The comparative example provides a preparation method of rhizoma smilacis glabrae extract, which adopts rhizoma smilacis glabrae decoction pieces in the same batch as in the example 1, and is different from the example 1 only in that the step S2 is replaced by reflux extraction for 2 times, the extraction time is 2 hours each time, the liquid medicine is obtained, the liquid medicine is kept to be slightly boiled in the reflux extraction process, and the temperature is about 100 ℃.
Comparative example 2
The comparative example provides a preparation method of rhizoma smilacis glabrae extract, which adopts rhizoma smilacis glabrae decoction pieces in the same batch as in the example 1, and is different from the example 1 only in that the step S2 is that the rhizoma smilacis glabrae decoction pieces are leached in water bath at the temperature of 80 ℃ for 2 times after boiling, and each time is 2 hours, so as to obtain liquid medicine.
Comparative example 3
The comparative example provides a preparation method of rhizoma smilacis glabrae extract, which adopts rhizoma smilacis glabrae decoction pieces in the same batch as in example 1, and is different from example 1 only in that the step S2 is replaced by directly leaching in water bath at 80 ℃ for 2 times, each time for 2 hours, so as to obtain liquid medicine.
Comparative example 4
The comparative example provides a preparation method of rhizoma smilacis glabrae extract, which adopts rhizoma smilacis glabrae decoction pieces in the same batch as in example 1, and is different from example 1 only in that the step S2 is replaced by water bath leaching for 2 times at 70 ℃ after boiling, and each time for 2 hours, so as to obtain liquid medicine.
Experimental example 1 solubility investigation
As the glabrous greenbrier rhizome extract still has precipitation after being added with hot water and stirred for 5min, the quantitative analysis of the precipitation amount and the dissolubility condition is difficult to observe by naked eyes. The method for calculating the insoluble matter ratio after suction filtration and drying precipitation can be used for quantitative analysis, but the time consumption is long and the process is complicated. The Turbocan analyzer can rapidly, accurately and quantitatively reflect the solubility and the precipitation condition of the sample through the change condition of the light intensity in the dissolution process of the smilax glabra extract, so the Turbocan analyzer is adopted for quantitative analysis of the solubility of the extract in the research.
The Turkiscan analyzer is based on multiple light scattering principle, and adopts two synchronous optical detectors of pulse near infrared light source (lambda=880 nm) and transmitted light and back scattered light to vertically scan the sample to be tested in the cylindrical glass test bottle from bottom to top. The transmission light detector receives the transmission light (T, 0 degree with the incident angle) transmitted through the sample and is used for researching a clear and transparent sample; the back-scattered light detector receives reflected light (BS, 135 ° from the angle of incidence) reflected by the sample for investigation of opaque samples up to 95% in concentration. The detector scans along the height of the sample (up to 55 mm), data of transmitted light and back scattered light are collected every 40 μm height, the data collection time can be set according to the change rate of the sample, and the data collection time can be collected every 0.1 second at the lowest. The curve obtained by scanning gives the change relation of the transmitted light and the back scattered light along with the height of the sample at different time points, and the change of the particle size and the dynamic changes of floating, sedimentation, aggregation/flocculation and the like of the particles in the sample can be intuitively, rapidly and accurately reflected. In addition, the Turkiscan also process data through Turbiscan Easysoft software to obtain parameters such as stability index (TSI), peak thickness and the like. When the phenomena of particle migration, precipitation and the like exist in the solution, the TSI value is increased along with the change of the transmission light and the back scattering light along with the particle migration speed, and the higher the TSI, the more unstable the solution is; peak thickness also increases with increasing thickness of the precipitate layer (see documents Huang Haozhou, lin Junzhi, wei Xichuan, ma Hongyan, liu Haiyan, fan Sanhu, wenquan, han Li, zhang Ding. Principles of pharmacy and regulation of stable storage of ellagic acid molecules in oral liquid of traditional Chinese medicine [ J ]. Pharmacology, 2019,54 (04): 737-745. And documents Hao-zhou Huang, sheng-yu Zhao, xiu-mei Ke, jun-zhi Lin, shu-sen Huang, run-chun Xu, hong-yan Ma, yi Zhang, li Han, ding-kun Zhang. Stud on the stability control strategy of Triphala solution based on the balance of physical stability and chemical stabilities [ J ]. Journal of Pharmaceutical and Biomedical Analysis,2018,158.).
Taking rhizoma smilacis glabrae extracts prepared in the examples and the comparative examples as test samples, respectively taking 1g of the test samples, heating 200mL of water, stirring for 5min, immediately pouring into a glass test bottle, and then putting into a scanning pool of a Turkiscan analyzer. The scanning is carried out every 30s along the vertical direction for 10min, and the transmission light curve data are obtained, and the result is shown in fig. 2. The scanned sample was then filtered through quantitative filter paper and the solids were dried to calculate the insoluble content (%), the insoluble content being the mass of the dried solids as a percentage of the mass of the test, and the results are shown in FIG. 3, example 1 being 4.03% and comparative examples 1-4 being 34.93%, 26.67%, 24.48%, 29.65%, respectively.
As a result, as shown in FIGS. 2 to 6, the glabrous greenbrier rhizome extract solution was transparent, and thus the transmitted light intensity (T) was selected for analysis. As can be seen from the time-varying patterns of the transmitted light intensities of the glabrous greenbrier rhizome extracts in FIG. 4, the transmitted light intensities of the sample solutions A to D are gradually increased along with the increase of time, the transmitted light intensities of the bottom (0-10 mm) and the top (30-40 mm) of the sample bottle are lower, the transmitted light intensities of the middle (10-30 mm) and the top (30-40 mm) are higher than the bottom, and the transmitted light intensities are gradually increased in a gradient manner, which indicates that the samples prepared in comparative examples 1-4 are precipitated at the bottom of the bottle, and the particles in the solution are continuously precipitated within 10min of standing, so that the solution from the middle to the top is gradually clarified. While the overall transmitted light intensity of fig. 4-E changed less, indicating that the sample prepared using example 1 was more stable and no significant precipitation occurred. Fig. 5 is a graph showing the trend of TSI values of five samples over time, and it can be seen that TSI values of all five samples gradually increase over time, but the TSI values of the samples prepared in example 1 have the smallest change, indicating that the stability is the best.
FIG. 6 shows the overall TSI at 10min, the average value of the light intensity at the top and bottom of the bottle, and the peak thickness of five samples calculated by Turbiscan Easysoft software, which accurately and quantitatively reflects the variation of each solution. In the graph, the average value of the top light intensity of the samples prepared in the comparative examples 1-4 is larger than 15%, the average value of the bottom light intensity is smaller than 0, and the average value of the top light intensity is obviously higher than the bottom; the average value of the light intensity at the top and bottom of the sample prepared in example 1 was about 2%, which is slightly different, further indicating that the samples prepared in comparative examples 1 to 4 had precipitation and poor solubility. The peak thickness reflects the height of the aqueous phase of the solution during delamination, the thicker the peak thickness, the thicker the thickness of the precipitate. As can be seen from the bottom peak thickness averages of the solutions in FIG. 6, the peak thickness averages of the sample solutions prepared using the extraction comparative examples 1, 2, 3, and 4 were all greater than 2mm, and comparative example 1 > comparative example 4 > comparative example 2 > comparative example 3, while the peak thickness averages of the sample solutions prepared using example 1 were almost 0, indicating that the samples prepared using example 1 had little or no precipitation, the samples prepared using comparative examples 1-4 had more precipitation, and the samples prepared using comparative example 1 had the most precipitation, followed by comparative example 4, comparative example 2, and comparative example 3.
It can be seen from the above-mentioned index that lowering the extraction temperature can improve the solubility of the smilax glabra extract, of which the solubility improvement of the smilax glabra extract of extraction example 1 is most remarkable.
Experimental example 2 characteristic Spectrum
Preparation of test solution: taking rhizoma Smilacis Glabrae extracts prepared in examples and comparative examples as test substances, grinding, respectively taking about 0.1g of test substances, placing into conical flask with plug, adding 70% ethanol 100mL, ultrasonic treating (power 300W, frequency 45 kHz) for 40min, taking out, cooling, shaking, filtering, and collecting filtrate.
Preparation of reference solution: 0.8010g of rhizoma Smilacis Glabrae reference material is taken, placed in a conical flask with a plug, added with 60% methanol 100mL, heated and refluxed for 60min, taken out, cooled, shaken uniformly, filtered, and the subsequent filtrate is taken as reference material solution of the reference material. And (3) taking proper amount of astilbin reference substance and engelhardin reference substance, precisely weighing, adding 60% methanol to prepare mixed solution containing astilbin 50.00 mug/mL and engelhardin 51.25 mug/mL, and taking as reference substance solution.
1. Mu.L of the reference solution and 1. Mu.L of the sample solution were aspirated, and the characteristic spectrum was measured under the following chromatographic conditions, with a ACQUITY UPLC HSS T C18 column (2.1 mm. Times.100 mm,1.8 μm); mobile phase: acetonitrile is taken as a mobile phase A, 0.2% glacial acetic acid solution is taken as a mobile phase B, and gradient elution is carried out; gradient elution conditions: 0-2 min,13% A; 2-5 min, 13-17% A; 5-14 min, 17-23% A; flow rate: 0.4mL min -1 The method comprises the steps of carrying out a first treatment on the surface of the Column temperature is 30 ℃; detection ofWavelength: 291nm; sample injection amount: 1 mul. The chromatogram and retention time were recorded. Matching the chromatograms by using a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2012A edition, and calculating the similarity between the UPLC chromatograms of the extracts and the reference map by taking the rhizoma smilacis glabrae reference medicinal material map (reference) as a reference, wherein the result is shown in figure 7.
Experimental results show that UPLC characteristic patterns of the rhizoma smilacis glabrae extract prepared by the five methods and the chromatogram of the reference substance of the reference medicinal material all detect 5 characteristic common peaks, and the similarity of the chromatograms is more than 0.96. And the retention time of astilbin peak and astragaloside peak in characteristic spectrum of each rhizoma smilacis glabrae extract corresponds to that of corresponding reference peak of reference substance, which shows that the components of each rhizoma smilacis glabrae extract have no obvious change, and the reduction of extraction temperature has no influence on the components.
Experimental example 3 astilbin content determination
Preparing a reference substance solution: taking proper amount of astilbin reference substance, precisely weighing, and adding 60% methanol to obtain reference substance solution containing astilbin 53.00 μg/mL.
Preparation of test solution: taking rhizoma smilacis glabrae extract prepared in the example and the comparative example as a test sample, grinding, respectively taking 0.1g of the test sample, precisely weighing, placing in a conical flask with a plug, precisely adding 100mL of 60% methanol, weighing, performing ultrasonic treatment (with the power of 300W and the frequency of 45 kHz) for 40min, cooling, weighing again, supplementing the lost weight with 60% methanol, shaking uniformly, and filtering with a 0.22 mu m filter membrane to obtain a test sample solution.
Respectively sucking the reference substance solution and the sample solution, and performing content measurement according to the following chromatographic conditions, wherein ACQUITY UPLC BEH C chromatographic column (2.1 mm×50mm,1.7 μm); mobile phase: methanol (a) -0.1% glacial acetic acid solution (B); elution conditions: 0-10 min:30% A; flow rate: 0.4 mL. ML -1 The method comprises the steps of carrying out a first treatment on the surface of the Column temperature: 30 ℃; detection wavelength: 291nm; sample injection amount: 2. Mu.L.
The content of astilbin in each group of smilax glabra extract and the transfer rate thereof (transfer rate of astilbin in smilax glabra extract=content of astilbin smilax glabra decoction piece extract/content of astilbin smilax glabra decoction piece) were calculated, and the peak positions of astilbin, and astilbin were identified according to the experimental results and with reference to national drug standard YBZ-PFKL-2021123 of the national drug administration, and the total flavone area was calculated, and the results are shown in the following table.
TABLE 1 astilbin content of rhizoma Smilacis Glabrae extract and transfer rate thereofn＝3)
Note that: total Huang Tongfeng area = new astilbin peak area + new alien astilbin peak area + alien astilbin peak area
Experimental results show that compared with comparative examples 1-4, the rhizoma smilacis glabrae extract obtained in the embodiment 1 of the invention has obviously improved astilbin content, transfer rate and total flavone content.
Experimental example 4 Multi-batch verification experiment
The extract was prepared by the method of example 1 from another 3 batches of glabrous greenbrier rhizome decoction pieces, and the falling solubility (insoluble matter ratio) was measured separately according to the above-described experiment, and the paste rate was calculated.
TABLE 2 extraction rates and insoluble content ratios of smilax glabra extract of different batchesn＝3)
| Numbering device | Paste yield (%) | Insoluble matter ratio |
| S2 | 17.09±0.28 | 6.9％ |
| S3 | 14.01±0.56 | 6.9％ |
| S4 | 14.70±0.60 | 6.4％ |
The results show that the smilax glabra extract prepared in the embodiment 1 has better dissolubility, and the extraction method can effectively improve the dissolubility of smilax glabra extract in different production areas and batches, and the paste yield meets the requirements of national drug standard YBZ-PFKL-2021123 (13% -24%) of the national drug administration.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A method for preparing rhizoma smilacis glabrae extract is characterized by comprising the steps of soaking rhizoma smilacis glabrae decoction pieces in water, performing water bath extraction at the temperature of 65-75 ℃ to obtain liquid medicine, filtering the liquid medicine, adding water for decoction, filtering, concentrating the filtrate, and drying.
2. The method for preparing a glabrous greenbrier rhizome extract according to claim 1, wherein the number of times of water bath extraction is 1-5, and the time of each water bath extraction is 2-4 hours; preferably, the number of times of water bath leaching is 2-3, and the time of each water bath leaching is 2.5-3.5h.
3. The method for preparing a smilax glabra extract according to claim 1 or 2, wherein the number of water bath leaches is 2 and the time of each water bath leaching is 2 hours.
4. A process for preparing a glabrous greenbrier rhizome extract according to any one of claims 1-3, wherein the temperature of the water bath leaching is 70 ℃.
5. The method for preparing a smilax glabra extract according to any one of claims 1 to 4, wherein the smilax glabra decoction pieces are soaked in water in an amount of 6 to 10 times the amount of water before water bath leaching.
6. The method for preparing rhizoma smilacis glabrae extract according to claim 5, wherein the soaking time is 20-40min.
7. The method for preparing a smilax glabra extract according to any one of claims 1 to 6, wherein the mass of water added in the water decoction process is 5 to 8 times the mass of smilax glabra decoction pieces, and the water decoction time is 2 to 4 hours.
8. The method for producing a smilax glabra extract according to any one of claims 1 to 7, wherein the ratio of the volume of the concentrated liquid medicine to the mass of smilax glabra decoction pieces is 1.5 to 2L:2kg.
9. A glabrous greenbrier rhizome extract produced by the method for producing a glabrous greenbrier rhizome extract of any one of claims 1 to 8.
10. A glabrous greenbrier rhizome formulation granule, characterized by comprising a glabrous greenbrier rhizome extract produced by the method for producing a glabrous greenbrier rhizome extract according to any one of claims 1 to 8.
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