CN106568909A - Quality control method of ludwigia hyssopifolia medicinal material - Google Patents
Quality control method of ludwigia hyssopifolia medicinal material Download PDFInfo
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Abstract
The invention discloses a quality control method of ludwigia hyssopifolia medicinal material. The quality control method mainly comprises steps of medicinal material characteristic identification and microscopic identification; and existing gallic acid content measuring and thin-layer identification are improved. The quality control method possesses relatively high specificity and reproducibility, can be used for evaluating the quality of ludwigia hyssopifolia medicinal material comprehensively, ensuring product quality of ludwigia hyssopifolia medicinal material, and providing scientific basis for standardization of ludwigia hyssopifolia medicinal material quality.
Description
Technical field
The invention belongs to Chinese medicinal material Quality Control Technology field, more particularly to a kind of quality control side of grass dragon medical material
Method.
Background technology
Careless dragon, also known as spire Herba Ludwigiae Prostratae, line leaf Herba Ludwigiae Prostratae, are Oenotheraceae grass dragon Ludwigia hyssopifolia
(G.Don) Exell is dried herb, is Zhuang nationality in Guangxi conventional Chinese herbal medicine among the people, with heat-clearing and toxic substances removing, putrefaction-removing granulation-promoting effect, uses
In treatment flu, laryngopharynx swelling and pain, sore scabies etc..It is among the people to have more significant curative effect using being proved the medicine, with applying valency well
Value.Careless dragon all herbal medicine, there is heat-clearing and toxic substances removing, removing the necrotic tissue and promoting granulation, can cure cold, laryngopharynx swelling and pain, sore scabies etc..《Guangxi book on Chinese herbal medicine
A collection of selected materials》、《Yunnan plant will》、《Hainan flora》、《Strong medicine a collection of selected materials》There is related record Deng books.Careless dragon originates in Chinese platform
Gulf, Guangdong, Hong Kong, Hainan, Guangxi, south of Yunnan, are born in the moistening area without shade such as field side, ditch, river shoal, the side of a pond, wet meadow, sea
50～750 meters are pulled out, India, Sri Lanka, Burma, the South East Asia Mainland Jing Malay Peninsulas to Philippine, Micronesia is distributed in
Northern with Australia, west is up to African torrid areas.
Careless dragon is more with all herbal medicine, and gallic acid, Palmic acid, isovanillin, cupreol, bean steroid are isolated in herb
Alcohol -3-O-B-D- glucosides, oleanolic acid, 2,4,6- trihydroxybenzoic acids, progallin A, ursolic acid, nimbecetin, people
The compounds such as ginseng saponin Rb1.Guangxi whole year among the people can harvest, and remove impurity, cutting, dry.At present grass dragon is with wild collection
Based on.At present about careless imperial pharmacological research mainly in antibiosis, research discovery, grass dragon Ethyl acetate extract and positive fourth
There are an obvious In Vitro Bacteriostasis at alcohol position, and it is Ethyl acetate extract that bacteriostasis are most strong.There is scholar to adopt agar dilution
Grass each extractive part of dragon and monomer component are determined to staphylococcus aureuses, staphylococcus epidermidiss, escherichia coli and green
The fungistatic effect of pus bacillus, it is found that the material of antibacterial action in grass dragon is present in and extract the larger position of polarity, i.e. ethyl acetate
Extract and n-butanol extract, and petroleum ether part does not have antibacterial activity, the antibacterial of chemical composition gallic acid is made in grass dragon
With working well.
The imperial distinctive drug effect of grass, as the conventional Chinese herbal medicine in Guangxi, has started in the market by extensive approval among the people
To careless dragon as health care medicine exploitation, but due to the method for quality control for having lacked, it is difficult to the quality of control grass dragon medical material, to just
Normal production and operation bring difficulty, it is therefore desirable to carry out specification to its method of quality control, to control the quality of careless dragon medical material.
At present, grass dragon medical material not yet sets up relevant criterion.Prior art only carries out indentification by TLC and efficient liquid phase to careless dragon medical material
The method of chromatography assay is imperfect, and specific aim is not strong, is difficult to reach real control quality of medicinal material using these methods
Purpose.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of science, complete, reliable, effectively grass dragon medical material quality control
Method processed.
To solve above-mentioned technical problem, the present invention is employed the following technical solutions：The method of quality control of careless dragon medical material, mainly
Differentiate including Medicinal Materials Characters and microscopical identification,
During Medicinal Materials Characters differentiate, in cylinder, lark is slightly bent, many fibrous roots, 0.3～0.8cm of diameter for medical material root；Stem
Surface celadon has thin vertical wrinkle to taupe, is in Dark grey at exfoliation, and matter is soft, and frangibility, section skin zone is thin, HUANGBAI(sic)
There is the marrow of broadness at color, woody part ivory buff, center；Leaf papery, lanceolar, place of wrinkling more, full edge has dilute pubescence, upper surface ash
Green, lower surface taupe, long 8～13cm, wide 2～5cm；Feeble QI, bitter in the mouth；Moisture must not exceed 15.0% in medical material, total ash
Divide and must not exceed 13.0%, acid-insoluble ash must not exceed 2.0%, and water-soluble extractivess must not be less than 10.0%；
In microscopical identification, medicinal powder is in yellow-white, and needle-like calcium oxalate crystal and cluster crystal are common, 28～71 μm of needle length, cluster crystal
15～28 μm of diameter；It can be seen that spiral duct or reticulate vessel, 6～23 μm of spiral duct diameter, 9～51 μm of reticulate vessel diameter；
There is a small amount of nonglandular hair, it is long 12～184 μm.
The method of quality control of above-mentioned grass dragon medical material, also differentiates, thin layer differentiates to adopt silica gel H lamellae including thin layer,
Using toluene-ethyl acetate-acetone-formic acid solution as developing solvent, with the mixing of the liquor ferri trichloridi of 1% potassium ferricyanide solution -1%
Solution is developer.
Thin layer differentiates to be carried out by following operation：The μ l of need testing solution 5, the μ l of reference substance solution 5 are taken, is put respectively in same silica gel
On H lamellaes, using the toluene-ethyl acetate-acetone-formic acid solution of volume ratio 5: 4: 0.5: 0.5 as developing solvent, launch, take
Go out, dry；With the mixed solution of the liquor ferri trichloridi of 1% potassium ferricyanide solution -1% of volume ratio 1: 1, daylight is inspected for spray；For
In test product chromatograph, on position corresponding with reference substance chromatograph, show the speckle of same color.
Medicinal powder 0.5g, as test sample, is taken with solution made by careless dragon herb medicinal powder, add water 20ml, supersound process
30 minutes, filtration, filtrate was evaporated, and methanol constant volume was added to 1ml, as need testing solution；Separately take gallic acid reference substance, plus first
Alcohol makes solution of every ml containing gallic acid 1mg.
It is above-mentioned grass dragon medical material method of quality control, also including assay, assay adopt mobile phase for methanol-
0.1% phosphoric acid mixed solution, 25 DEG C of column temperature, Detection wavelength is 272nm.
Assay is carried out by following operation：With octadecylsilane chemically bonded silica as filler；With volume ratio 1: 99
The phosphoric acid of methanol -0.1% mixed solution is mobile phase；25 DEG C of column temperature, Detection wavelength is 272nm；Number of theoretical plate presses gallic acid peak
Calculating should be not less than 2000；It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, chromatograph of liquid is injected, survey
It is fixed, obtain final product.
Precision claims gallic acid reference substance appropriate, adds water and makes solution of every 1ml containing the μ g of gallic acid 30, obtains final product reference substance
Solution；Medicinal powder (crossing No. four sieves) 0.2g is taken, accurately weighed, in putting tool plug round-bottomed flask, precision adds 10% hydrochloric acid solution
25ml, weighed weight is put and be heated to reflux in water-bath 30mim, is let cool, then weighed weight, and with 10% hydrochloric acid the weight of less loss is supplied,
Shake up, filter, take subsequent filtrate, obtain final product need testing solution.
Lack the problem of related quality criterion at present grass dragon medical material, inventor on the basis of prior art means,
Through long-term in-depth study, a kind of science, complete, reliable, effectively grass dragon medical material method of quality control are established, mainly
Differentiate (moisture content, ash and extractum) and microscopical identification including Medicinal Materials Characters, also improve existing gallic acid content and survey
Fixed and thin layer differentiates.The method has stronger specificity and good repeatability, can thoroughly evaluating grass dragon quality of medicinal material, effectively guarantor
The product quality of card grass dragon medical material, for specification grass dragon quality of medicinal material scientific basis is provided.
Description of the drawings
Fig. 1 is the structural map (× 400) of careless dragon powder, in figure：1 needle, 2 reticulate vessels, 3 spiral ducts, 4 pores, 5 is non-
Glandular hair, 6 cluster crystals.
Fig. 2 is the cross section structural map of careless dragon root, in figure：1 withered epidermis, 2 cortexes, 3 phloems, 4 cambium layer, 5 lead
Pipe, 6 xylem ray, 7 primary xylems.
Fig. 3 is the cross section structural map of careless dragon stem, in figure：1 epidermis, 2 cortexes, 3 phloem fibers, 4 phloems, 5 is wooden
Portion, 6 cluster crystals, 7 marrows.
Fig. 4 is the cross section structural map of careless dragon leaf, in figure：1 epidermis, 2 palisade tissues, 3 phloem fibers, 4 phloems, 5
Xylem, 6 cluster crystals, 7 marrows.
Fig. 5 is the thin layer discriminating figure of 11 kinds of different sources grass dragons, in figure：1-11 is respectively the grass dragon of 1#-11# different sources
Medical material；12nd, gallic acid reference substance.
Fig. 6 is HPLC figures, in figure：A reference substances, B test samples, C negative controls.
Specific embodiment
Grass dragon medical material is from 11 different sources, Jing Guangxi national medicine academy Huang Ruisong researcher used by following example
Be accredited as Oenotheraceae grass dragon Ludwigia hyssopifolia (G.Don) Exell is dried herb.Crude drug source is believed in detail
Breath is shown in Table 1.
The different sources of table 1 grass dragon numbering
The character identification of embodiment 1
The character of the grass dragon medical material from 11 different sources is differentiated, is as a result shown：Careless dragon medical material root is in cylinder
Shape, lark is slightly bent, many fibrous roots, 0.3～0.8cm of diameter；Stem surface celadon has thin vertical wrinkle to taupe, and epidermis takes off
Place fall in Dark grey, matter is soft, and frangibility, section skin zone is thin, yellow-white, woody part ivory buff, there is the marrow of broadness at center；Leaf paper
Matter, lanceolar, place of wrinkling more, full edge has dilute pubescence, upper surface celadon, lower surface taupe, long 8～13cm, wide 2～5cm；
Feeble QI, bitter in the mouth.
The microscopical identification (Fig. 1 to Fig. 4) of embodiment 2
Microstructure to the grass dragon medical material from 11 different sources is differentiated, is as a result shown：Medicinal powder is in Huang
White, needle-like calcium oxalate crystal and cluster crystal it is common, 28～71 μm of needle length, 15～28 μm of cluster crystal diameter；It can be seen that spiral duct or reticulate pattern
Conduit, 6～23 μm of spiral duct diameter, 9～51 μm of reticulate vessel diameter；There is a small amount of nonglandular hair, it is long 12～184 μm.
To sum up, the microscopical identification main points system of grass dragon medical material：Powder calcium oxalate crystal growth in healthy needle is numerous, some clusters, long 15～75 μ
m.Calcium oxalate cluster crystal Flos Chrysanthemi shape, about 25 μm of diameter.
Additionally, inventor has also carried out root cross section, stem cross section, the cross section micro- sight of leaf to all grass dragon medical materials
Examine, it is as a result as follows：
Root cross section (Fig. 2) --- in subcircular, phellem layer is made up of 5-7 row flat, rectangular cells, marshalling.Dimension
The unlimited outer tough radial arrangement cyclization of tubing string.Vascular ray is obvious；Xylem differentiation to center, without marrow, but xylem parenchyma
It is more, visible needle-like calcium oxalate crystal in parenchyma cell.
Stem cross section (Fig. 3) --- in partially circular.Epidermis has thicker horny layer；Cortex is narrower, and vascular bundle is unlimited outer tough
Type radial arrangement cyclization；Phloem is narrower, and outside has more phloem fiber, and often aggregation bunchy constitutes interrupted concentric ring, shape
About 2 layers of stratification；Xylem vessel is single or in column, and wood fiber cell is more, and vascular ray is obvious；Marrow is larger, and marrow is scattered
Calcium oxalate cluster crystal.
Leaf cross section (Fig. 4) --- up and down epidermis cell each 1 is arranged, and cell similar round has a small amount of nonglandular hair；Mesophyll tissue point
Change substantially, palisade tissue 1 is arranged, cell shape is in long cylindricality, not by master pulse；Sponge is organized by the thin of similar round or long cylindricality
Parietal cell is constituted, and arranges loose, there is obvious intercellular substance, has a large amount of cluster crystals and a small amount of needle.The upper and lower epidermis inner side tool of vein is thick
Angled tissue.Vascular bundle similar round, outer tough type, cambium layer is not obvious, common cluster crystal, mesophyll tissue in blade middle arteries and mesophyll tissue
In be rich in raphides.
The thin-layer chromatographic analysis of embodiment 3
Medicinal powder 0.5g, as test sample, is taken with solution made by careless dragon herb medicinal powder, add water 20ml, supersound process
30 minutes, filtration, filtrate was evaporated, and methanol constant volume was added to 1ml, as need testing solution；Separately take gallic acid reference substance, plus first
Alcohol makes solution of every ml containing gallic acid 1mg.According to thin layer chromatography (《Chinese Pharmacopoeia》One annex VI B of version in 2010)
Experiment, takes the μ l of need testing solution 5, the μ l of reference substance solution 5, puts respectively on same silica gel H lamellae, with toluene-ethyl acetate-
Acetone-formic acid solution (5: 4: 0.5: 0.5) launches as developing solvent, takes out, and dries；Spray is with 1% potassium ferricyanide solution -1% three
The mixed solution of ferric chloride solution (1: 1), daylight is inspected.
11 batches of medical material samples are determined, as a result as shown in figure 5, in test sample chromatograph, in position corresponding with reference substance chromatograph
On, show the speckle of same color, also illustrate TLC methods repeatability preferably.
The inspection of the moisture of embodiment 4, total ash, acid insoluble ash and extractum
Different sources grass dragon medical material (crossing No. 2 sieves) about 2.0g is taken, according to《Chinese Pharmacopoeia》One determination of water of version in 2010
Oven drying method (annex IX the first methods of H) is determined under method item.Careless dragon about 2g is taken, is laid in and is dried into the flat weighing bottle of constant weight, thickness
Less than 5mm, loose test sample is less than 10mm, accurately weighed, bottle cap is opened in 100～105 DEG C of dryings 5 hours, by bottle cap
Cover, in moving to exsiccator, cool down 30 minutes, accurately weighed weight, then be dried 1 hour in said temperature, cooling is weighed, extremely
The double difference weighed is less than till 5mg.According to the weight of less loss, water content (%) in test sample is calculated.As a result see
Table 2.
The grass dragon sample moisture measurement result of table 2
As a result show, between 9.0～12.6%, it is average aqueous to be divided into 10.4% to 11 batches of sample moisture contents.Therefore draft
This product standard aqueous point must not exceed 15.0%.
Total ash is determined：Reference《Chinese Pharmacopoeia》(1. total ash is determined the one annex IX K Ash determination method of version in 2010
Method) total ash is carried out to 11 batches of samples it is measured.Different sources grass dragon medical material (crossing No. 2 sieves) about 4.0g is taken, according to《Middle traditional Chinese medicines
Allusion quotation》Total ash algoscopy (annex IX K) is determined under the one Ash determination method item of version in 2010.The sample of measure must be crushed, and be made
2～3g of sample (as acid-insoluble ash must be determined, can use and supply 3～5g of sample) can be taken by No. two sieves, after mix homogeneously, be put
In the crucible of ignition to constant weight, weighed weight (accurately to 0.01) is slowly scorching hot, notes avoiding burning, when complete carbonization, by
High-temperature edge up to 500～600 DEG C, makes to be ashed completely to constant weight.According to residue weight, the content of total ash in sample is calculated
(%).The results are shown in Table 3.
The grass dragon sample total ash measurement result of table 3
As a result show, 4.4%～12.7%, average total ash content is 7.8% to 11 batches of sample total ashs.Therefore intend regulation
This product standard total ash must not cross 13.0%.
Acid insoluble ash：Reference《Chinese Pharmacopoeia》The one annex IX K Ash determination method of version in 2010 (2. acid insoluble ash
Algoscopy) 11 batches of samples are measured.According to《Chinese Pharmacopoeia》Sour insoluble ash under the one Ash determination method item of version in 2010
Algoscopy (annex IX K) is divided to determine.The ash obtained by item is taken, notes adding dilute hydrochloric acid about 10ml in crucible, use surface plate
Crucible is covered, is put and heated 10 minutes in water-bath, surface plate is rinsed with hot water 5ml, and washing liquid is incorporated in crucible, is filtered with ashless filter paper
Cross, the residue in crucible is washed with water on filter paper, and washing chloride reaction aobvious to washing liquid.Filtrate moves to together with filter paper
In same crucible, it is dried, ignition to constant weight.According to residue weight, acid-insoluble ash weight (%) in test sample is calculated.As a result
It is shown in Table 4.
The grass dragon sample acid-insoluble ash measurement result of table 4
According to said determination result, between 0.1%～1.5%, average acid is or not 11 batches of sample acid-insoluble ash contents
Dissolubility content of ashes is 0.6%.Therefore intend regulation this product standard acid-insoluble ash and must not exceed 2.0%.
Extractum according to《Chinese Pharmacopoeia》One hot dipping of version in 2010 is determined.Test sample about 2～4g is taken, it is accurately weighed,
In putting the conical flask of 100～250ml, precision adds water 50～100ml, close plug, weighed weight, after standing 1 hour, connects returned cold
Solidifying pipe, is heated to boiling, and keeps micro-boiling 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, supplied with water and subtracted
The weight of mistake, shakes up, and is filtered with exsiccator, and precision measures filtrate 25ml, puts and be dried into the evaporating dish of constant weight, in water-bath
After being evaporated, in 105 DEG C of dryings 3 hours, put in exsiccator and cool down 30 minutes, rapid accurately weighed weight.Unless otherwise specified, with
Dry product calculates the content (%) of water-soluble extractivess in test sample.The results are shown in Table 5.
The grass dragon sample determination of extractives result of table 5
According to said determination result, between 10.3%～34.2%, average extractum is 11 batches of sample extractum
21.6%.In view of the difference of crude drug source, therefore this product standard extract content is drafted no less than 10.0%.
The assay of embodiment 5
First, instrument and material
LC-20AT high performance liquid chromatographs (band automatic sampler) diode array detector, LCsolution chromatograph works
Stand (be Japanese Shimadzu Corporation)；KQ-100.DE type numerical control ultrasonic cleaners (Kunming Ultrasound Instrument company limited)；X205
BDU electronic analytical balances (Mei Tele companies of Switzerland)；EASY PURE II Superpure water machines (power ＆ light company of the U.S.) etc..Gallic acid
Reference substance (Chengdu Man Site bio tech ltd, content：98%, lot number：MUST-13040103)；First used by mobile phase
Alcohol is chromatographically pure (Fisher companies of the U.S.), water is ultra-pure water, and it is pure that remaining is analysis.
2nd, method
With octadecylsilane chemically bonded silica as filler, chromatographic column is Gemini C18(4.6mm × 250mm, 5 μm)；With
The phosphoric acid of methanol -0.1% (1: 99) is mobile phase；25 DEG C of column temperature, Detection wavelength is 272nm.Number of theoretical plate is based on gallic acid peak
Calculation should be not less than 2000.Precision claims gallic acid reference substance appropriate, adds water and makes solution of every 1ml containing the μ g of gallic acid 30, i.e.,
Obtain reference substance solution.This product powder (crossing No. four sieves) 0.2g is taken, accurately weighed, in putting tool plug round-bottomed flask, precision adds 10%
Hydrochloric acid solution 25ml, weighed weight is put and be heated to reflux in water-bath 30mim, is let cool, then weighed weight, is supplied with 10% hydrochloric acid and is subtracted
The weight of mistake, shakes up, and filters, and takes subsequent filtrate and obtains final product need testing solution.It is accurate respectively to draw reference substance solution and need testing solution
Each 10 μ l, inject chromatograph of liquid, determine, and obtain final product.
As a result：Need testing solution and according on the corresponding position of product solution chromatogram, time identical chromatographic peak of withing a hook at the end, and
Negative controls chromatogram is then without this chromatographic peak.See Fig. 6.
1>Linear relationship is investigated
Take gallic acid reference substance appropriate, add water and make the solution of 0.5mg/ml, it is accurate respectively to draw 0.2,1,2,3,4,
5ml, respectively adds water and is settled to 5ml, shakes up.It is accurate respectively to draw each 10 μ l of above-mentioned need testing solution, HPLC is injected, with gallic acid
Peak area is vertical coordinate, and sample size (μ g) is abscissa, draws standard curve.Obtain the regression equation of gallic acid：Y=
2770704.84x-89286, r=0.9999, gallic acid is in good line with peak area in 0.1974～4.935 μ g ranges
Sexual intercourse.
2>Precision test
Same need testing solution is taken, is determined 5 times by above-mentioned chromatographic condition continuous sample introduction.As a result：Determine gallic acid peak 5 times
The RSD=0.54% of area.Show that instrument precision is good.
3>Replica test
6 parts of same sample powder is taken, every part of 0.2g is accurately weighed, prepares need testing solution, surveyed by above-mentioned chromatographic condition
It is fixed.As a result：The RSD of gallic acid content is 1.30% in 6 parts of need testing solutions.Show that this method repeatability is good.
4>Stability test
Same need testing solution is taken, by above-mentioned chromatographic condition, respectively at 1,2,4,8,12,24h sample introductions are determined.As a result：Sample
The RSD of gallic acid peak area is 0.85% in product.Show that the gallic acid in need testing solution is good in the internal stability of 24h
It is good.
5>Average recovery is tested
6 parts of known content same sample powder is taken, each 0.1g is accurately weighed, precision adds gallic acid reference substance solution
(68 μ g/ml) 25ml, prepares need testing solution, by above-mentioned chromatographic condition determine gallic acid content, calculate average recovery rate and
RSD.As a result：It is 97.54%, RSD=1.99% to determine gallic acid content average recovery rate.
3rd, sample determination
Reference《Chinese Pharmacopoeia》2010 editions annex VI D high performance liquid chromatography, according to the method described above to 11 batch medicines
Material sample is measured, and the results are shown in Table 6.
The sample size measurement result (n=2) of table 6
As a result show：11 batches of sample gallic acid contents are 0.69%～5.14%, and average content is 2.61%.According to 11
Criticize the measurement result of sample, it is contemplated that crude drug source difference condition, draft this product standard and calculate containing gallic acid by dry product
(C7H6O5) 0.50% must not be less than.
Claims (7)
1. a kind of method of quality control of grass dragon medical material, it is characterised in that mainly include that Medicinal Materials Characters differentiate and microscopical identification, institute
In stating Medicinal Materials Characters discriminating, in cylinder, lark is slightly bent, many fibrous roots, 0.3～0.8cm of diameter for medical material root；Stem surface ash
Green has thin vertical wrinkle to taupe, is in Dark grey at exfoliation, and matter is soft, and frangibility, section skin zone is thin, yellow-white, woody part
There is the marrow of broadness at ivory buff, center；Leaf papery, lanceolar, place of wrinkling more, full edge has dilute pubescence, upper surface celadon, under
Surface taupe, long 8～13cm, wide 2～5cm；Feeble QI, bitter in the mouth；Moisture must not exceed 15.0% in medical material, and total ash must not surpass
13.0% is crossed, acid-insoluble ash must not exceed 2.0%, and water-soluble extractivess must not be less than 10.0%；
In the microscopical identification, medicinal powder is in yellow-white, and needle-like calcium oxalate crystal and cluster crystal are common, 28～71 μm of needle length, cluster crystal
15～28 μm of diameter；It can be seen that spiral duct or reticulate vessel, 6～23 μm of spiral duct diameter, 9～51 μm of reticulate vessel diameter；
There is a small amount of nonglandular hair, it is long 12～184 μm.
2. it is according to claim 1 grass dragon medical material method of quality control, it is characterised in that also including thin layer differentiate, thin layer
Differentiate to adopt silica gel H lamellae, it is molten with 1% potassium ferricyanide using toluene-ethyl acetate-acetone-formic acid solution as developing solvent
The liquor ferri trichloridi of liquid -1% mixed solution is developer.
3. it is according to claim 2 grass dragon medical material method of quality control, it is characterised in that thin layer differentiate press following operation
Carry out：The μ l of need testing solution 5, the μ l of reference substance solution 5 are taken, are put respectively on same silica gel H lamellae, with volume ratio 5: 4: 0.5:
0.5 toluene-ethyl acetate-acetone-formic acid solution launches as developing solvent, takes out, and dries；Spray is with the 1% of volume ratio 1: 1
The mixed solution of the liquor ferri trichloridi of potassium ferricyanide solution -1%, daylight is inspected；In test sample chromatograph, with reference substance chromatograph phase
On the position answered, show the speckle of same color.
4. it is according to claim 3 grass dragon medical material method of quality control, it is characterised in that：With careless dragon herb medicinal powder
Made by solution be test sample, take medicinal powder 0.5g, add water 20ml, supersound process 30 minutes, filtration, and filtrate is evaporated, and adds
Methanol constant volume to 1ml, as need testing solution；Gallic acid reference substance is separately taken, plus methanol makes every ml and contains gallic acid 1mg's
Solution.
5. it is according to claim 1 grass dragon medical material method of quality control, it is characterised in that also including assay, content
Measure adopts mobile phase for the phosphoric acid mixed solution of methanol -0.1%, 25 DEG C of column temperature, and Detection wavelength is 272nm.
6. it is according to claim 5 grass dragon medical material method of quality control, it is characterised in that assay press following operation
Carry out：With octadecylsilane chemically bonded silica as filler；With the phosphoric acid of methanol -0.1% mixed solution of volume ratio 1: 99 as stream
Dynamic phase；25 DEG C of column temperature, Detection wavelength is 272nm；Number of theoretical plate is calculated by gallic acid peak and should be not less than 2000；It is accurate respectively to inhale
Reference substance solution and each 10 μ l of need testing solution are taken, chromatograph of liquid is injected, is determined, obtained final product.
7. it is according to claim 6 grass dragon medical material method of quality control, it is characterised in that：Precision claims gallic acid control
Appropriate product, add water and make solution of every 1ml containing the μ g of gallic acid 30, obtain final product reference substance solution；Medicinal powder 0.2g is taken, precision claims
Fixed, in putting tool plug round-bottomed flask, precision adds 10% hydrochloric acid solution 25ml, weighed weight to put and be heated to reflux in water-bath 30mim,
Let cool, then weighed weight, the weight of less loss is supplied with 10% hydrochloric acid, shake up, filter, subsequent filtrate is taken, obtain final product need testing solution.
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| CN111983060A (en) * | 2020-08-03 | 2020-11-24 | 广西国际壮医医院 | Quality control method of wild six-cereal medicinal material |
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