CN106568909B - The method of quality control of careless dragon medicinal material - Google Patents
The method of quality control of careless dragon medicinal material Download PDFInfo
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Abstract
The invention discloses a kind of method of quality control of the imperial medicinal material of grass, mainly include Medicinal Materials Characters identification and microscopical characters, also improve existing gallic acid content measurement and thin layer identifies.The method has stronger specificity and good reproducibility, can the imperial quality of medicinal material of thoroughly evaluating grass, the product quality of careless imperial medicinal material is effectively ensured, provides scientific basis for the imperial quality of medicinal material of specification grass.
Description
Technical field
The invention belongs to Chinese medicinal material quality control technology more particularly to a kind of quality controlling parties of the imperial medicinal material of grass
Method.
Background technique
Careless dragon also known as spire climbing seedbox herb, line leaf false loosestrife are Oenotheraceae grass dragon Ludwigia hyssopifolia
(G.Don) the drying herb of Exell is the civil common Chinese herbal medicine of Zhuang nationality in Guangxi, has effects that clearing heat and detoxicating, putrefaction-removing granulation-promoting, is used
In treatment flu, abscess of throat, sore scabies etc..Civil use, which is proved the medicine, more significant curative effect, has and applies valence well
Value.Careless dragon all herbal medicine, there is the effect of clearing heat and detoxicating, to remove necrosis and promote granulation, and can cure cold, abscess of throat, sore scabies etc.." Guangxi book on Chinese herbal medicine
A collection of selected materials ", " Yunnan plant will ", " Hainan flora ", the books such as " strong medicine a collection of selected materials " have related record.Careless dragon originates in Taiwan, wide
East, Hong Kong, Hainan, Guangxi, south of Yunnan are born in the wet area without shade such as field side, ditch, river shoal, the side of a pond, wet meadow, height above sea level 50
~750 meters, India, Sri Lanka, Burma, South East Asia Mainland are distributed in through the Malay Peninsula to Philippine, Micronesia and Australia
Big Leah is northern, and west reaches African torrid areas.
Careless dragon isolates gallic acid, palmitinic acid, isovanillin, cupreol, beans steroid in herb mostly with all herbal medicine
Alcohol -3-O-B-D- glucoside, oleanolic acid, 2,4,6- trihydroxybenzoic acids, progallin A, ursolic acid, Kaempferol, people
Join the compounds such as saponin(e Rb1.Guangxi civil whole year can harvest, and remove impurity, dissection, dry.Grass dragon is at present with wild acquisition
Based on.Pharmacological research at present in relation to careless dragon is mainly in antibiosis, the study found that grass dragon Ethyl acetate extract and positive fourth
There is apparent In Vitro Bacteriostasis at alcohol position, and strongest bacteriostasis is Ethyl acetate extract.There is scholar using agar dilution
The measurement grass each extractive part of dragon and monomer component are to staphylococcus aureus, staphylococcus epidermis, escherichia coli and green
The fungistatic effect of purulence bacillus finds that the substance of antibacterial action in grass dragon is present in and extracts the biggish 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 component gallic acid is made in grass dragon
With working well.
The careless distinctive drug effect of dragon has been started by civil extensive approval as the common Chinese herbal medicine in Guangxi currently on the market
Careless dragon is developed as health medicine, but the method for quality control due to having lacked, it is difficult to the quality of the imperial medicinal material of control grass, to just
Normal production and operation bring difficulty, it is therefore desirable to standardize to its method of quality control, to control the quality of the imperial medicinal material of grass.
Currently, grass dragon medicinal material not yet establishes relevant criterion.The prior art only carries out indentification by TLC and efficient liquid phase to careless imperial medicinal 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.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of science, the quality control of complete, reliable, the effective imperial medicinal material of grass
Method processed.
In order to solve the above technical problems, the invention adopts the following technical scheme: grass dragon medicinal material method of quality control, mainly
Including Medicinal Materials Characters identify and microscopical characters,
During Medicinal Materials Characters identify, medicinal material root is cylindrical, and lark is slightly bent, pogoniasis root, 0.3~0.8cm of diameter；Stem
Surface celadon has thin vertical wrinkle, is in Dark grey at excoriation, matter is soft, frangibility, and section skin zone is thin, yellowish-white to taupe
There is wide marrow at color, woody part ivory buff, center；Leaf papery, lanceolar, more shrinkages, full edge have dilute pubescence, upper surface ash
Green, lower surface taupe, long 8~13cm, wide 2~5cm；Gas is micro-, bitter；Moisture must not exceed 15.0% in medicinal material, total ash
Divide and must not exceed 13.0%, acid-insoluble ash must not exceed 2.0%, and water-soluble extractives must not be lower than 10.0%；
In microscopical characters, medicinal powder is in yellow-white, and needle-like calcium oxalate crystal and cluster crystal are common, and needle is 28~71 μm long, 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 12~184 μm long.
The method of quality control of the imperial medicinal material of above-mentioned grass further includes that thin layer identifies, and thin layer, which identifies, uses silica gel H lamellae,
Using toluene-ethyl acetate-acetone-formic acid solution as solvent, with the mixing of -1% liquor ferri trichloridi of 1% potassium ferricyanide solution
Solution is color developing agent.
Thin layer identifies to be carried out by following operation: 5 μ l of test solution, 5 μ l of reference substance solution being taken to be put respectively in same silica gel
On H lamellae, using toluene-ethyl acetate-acetone-formic acid solution of volume ratio 5:4:0.5:0.5 as solvent, expansion,
It takes out, dries；With the mixed solution of -1% liquor ferri trichloridi of 1% potassium ferricyanide solution of volume ratio 1:1, daylight is inspected for spray；
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
Using solution made of careless imperial herb medicinal powder as test sample, medicinal powder 0.5g is taken, water 20ml is added, is ultrasonically treated
30 minutes, filtration, filtrate was evaporated, and methanol constant volume is added to 1ml, as test solution；Gallic acid reference substance separately is taken, adds first
The solution of every ml 1mg containing gallic acid is made in alcohol.
The method of quality control of the above-mentioned imperial medicinal material of grass, further includes assay, assay uses mobile phase for methanol-
0.1% phosphoric acid mixed solution, 25 DEG C of column temperature, Detection wavelength 272nm.
Assay is carried out by following operation: using octadecylsilane chemically bonded silica as filler；With volume ratio 1:99's
- 0.1% phosphoric acid mixed solution of methanol is mobile phase；25 DEG C of column temperature, Detection wavelength 272nm；Number of theoretical plate presses gallic acid peak
2000 should be not less than by calculating；It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is surveyed
It is fixed to get.
Precision claims gallic acid reference substance appropriate, adds water that the solution of every 1ml 30 μ g containing gallic acid is made to get reference substance
Solution；Medicinal powder (crossing No. four sieves) 0.2g is taken, it is accurately weighed, it sets in tool plug round-bottomed flask, 10% hydrochloric acid solution is added in precision
25ml, weighed weight, sets and is heated to reflux 30mim in water-bath, lets cool, then weighed weight, and the weight of less loss is supplied with 10% hydrochloric acid,
It shakes up, filters, take subsequent filtrate to get test solution.
Aiming at the problem that the current imperial medicinal material of grass lacks related quality criterion, inventor on the basis of prior art means,
By long-term in-depth study, a kind of method of quality control of scientific, complete, reliable, effective grass dragon medicinal material is established, mainly
Identify (moisture content, ash content and extract) and microscopical characters including Medicinal Materials Characters, also improves existing gallic acid content and survey
Fixed and thin layer identifies.The method has stronger specificity and good reproducibility, can the imperial quality of medicinal material of thoroughly evaluating grass, effectively guarantor
The product quality of the imperial medicinal material of card grass provides scientific basis for the imperial quality of medicinal material of specification grass.
Detailed description of the invention
Fig. 1 is the structural map (× 400) of careless imperial powder, and in figure: 1 needle, 2 reticulate vessels, 3 spiral ducts, 4 stomatas, 5 is non-
Glandular hairs, 6 cluster crystals.
Fig. 2 is the structural map in careless imperial root cross section, and in figure: 1 withered epidermis, 2 cortexes, 3 basts, 4 forming layers, 5 lead
Pipe, 6 wood radiaftive rays, 7 primary xylems.
Fig. 3 is the structural map in careless imperial stem cross section, and in figure: 1 epidermis, 2 cortexes, 3 phloem fibers, 4 basts, 5 is wooden
Portion, 6 cluster crystals, 7 marrows.
Fig. 4 is the structural map in careless imperial leaf cross section, in figure: 1 epidermis, 2 palisade tissues, 3 phloem fibers, 4 basts, 5
Xylem, 6 cluster crystals, 7 marrows.
Fig. 5 is the thin layer identification figure of 11 kinds of different sources grass dragon, and in figure: 1-11 is the grass dragon of 1#-11# different sources respectively
Medicinal material；12, gallic acid reference substance.
Fig. 6 is that HPLC schemes, in figure: A reference substance, B test sample, C negative control.
Specific embodiment
The dragon medicinal material of grass used in following example comes from 11 different sources, through Guangxi national medicine research institute Huang Ruisong researcher
It is accredited as the drying herb of Oenotheraceae grass dragon Ludwigia hyssopifolia (G.Don) Exell.Crude drug source is believed in detail
Breath is shown in Table 1.
Table 1 different sources grass dragon number
1 character of embodiment identifies
The character of the imperial medicinal material of grass from 11 different sources is identified, as the result is shown: grass dragon medicinal material root is in cylinder
Shape, lark is slightly bent, pogoniasis root, 0.3~0.8cm of diameter；Stem surface celadon has thin vertical wrinkle, epidermis is de- to taupe
Place is fallen in Dark grey, matter is soft, frangibility, and section skin zone is thin, yellow-white, and there is wide marrow at woody part ivory buff, center；Leaf paper
Matter, lanceolar, more shrinkages, full edge have dilute pubescence, upper surface celadon, lower surface taupe, long 8~13cm, wide 2~5cm；
Gas is micro-, bitter.
2 microscopical characters of embodiment (Fig. 1 to Fig. 4)
The microstructure of the imperial medicinal material of grass from 11 different sources is identified, as the result is shown: medicinal powder is in Huang
White, needle-like calcium oxalate crystal and cluster crystal are common, and needle is 28~71 μm, 15~28 μm of cluster crystal diameter long；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 12~184 μm long.
To sum up, the microscopical characters main points system of the imperial medicinal material of grass: powder calcium oxalate crystal growth in healthy needle is numerous, some clusters, long 15~75 μ
m.Calcium oxalate cluster crystal chrysanthemum shape, about 25 μm of diameter.
In addition, inventor has also carried out the micro- sight in root cross section, stem cross section, leaf cross section to the imperial medicinal material of all grass
It examines, as a result as follows:
Root cross section (Fig. 2) --- it is in subcircular, phellem layer is made of 5-7 column flat, rectangular cell, marshalling.Dimension
The unlimited outer tough radial arrangement cyclization of tubing string.Vascular ray is obvious；Xylem differentiation is to center, no marrow, but wood-parenchymatous cell
It is more, visible needle-like calcium oxalate crystal in parenchyma cell.
Stem cross section (Fig. 3) --- in partially round.Epidermis has thicker cuticula；Cortex is relatively narrow, and vascular bundle is unlimited outer tough
Type radial arrangement cyclization；Bast is relatively narrow, and outside has more bast fiber, often gathers into bundles and constitutes interrupted concentric ring, shape
About 2 layers of stratification；Individually or in column, wood-fibred cell is more, and vascular ray is obvious for xylem vessel；Marrow is larger, and marrow is scattered
Calcium oxalate cluster crystal.
Leaf cross section (Fig. 4) --- upper and lower each 1 column of epidermal cell, cell similar round have a small amount of nonglandular hair；Mesophyll tissue point
Change obviously, palisade tissue 1 arranges, and cell shape is in long cylindricality, does not pass through master pulse；Sponge tissue is by similar round or long cylindrical thin-walled
Cell composition, arrangement is loose, has obvious space between cells, has a large amount of cluster crystals and a small amount of needle.Has thick angle on the inside of the upper and lower epidermis of vein
Tissue.Vascular bundle similar round, outer tough type, forming layer is unobvious, common cluster crystal in blade middle arteries and mesophyll tissue, in mesophyll tissue
Rich in raphides.
3 thin-layer chromatographic analysis of embodiment
Using solution made of careless imperial herb medicinal powder as test sample, medicinal powder 0.5g is taken, water 20ml is added, is ultrasonically treated
30 minutes, filtration, filtrate was evaporated, and methanol constant volume is added to 1ml, as test solution；Gallic acid reference substance separately is taken, adds first
The solution of every ml 1mg containing gallic acid is made in alcohol.It is real according to thin-layered chromatography (one VI B of annex of " Chinese Pharmacopoeia " version in 2010)
It tests, takes 5 μ l of test solution, 5 μ l of reference substance solution, put respectively on same silica gel H lamellae, with toluene-ethyl acetate-
Acetone-formic acid solution (5:4:0.5:0.5) is used as solvent, is unfolded, and takes out, dries；Spray is with 1% potassium ferricyanide solution -1%
The mixed solution of liquor ferri trichloridi (1:1), daylight are inspected.
11 batches of medicinal material samples are measured, as a result as shown in figure 5, in sample chromatogram, in position corresponding with reference substance chromatography
On, the spot of same color is shown, also illustrates TLC method repeatability preferably.
The inspection of embodiment 4 moisture, total ash, acid insoluble ash and extract
The imperial medicinal material of different sources grass (crossing No. 2 sieves) about 2.0g is taken, according to one determination of moisture of " Chinese Pharmacopoeia " version in 2010
Oven drying method (Ⅸ the first method of H of annex) measures under method item.Careless dragon about 2g is taken, dry into the flat weighing bottle of constant weight, thickness is laid in
No more than 5mm, loose test sample is no more than 10mm, and accurately weighed, opening bottle cap is 5 hours dry at 100~105 DEG C, by bottle cap
It covers, moves in drier, 30 minutes cooling, accurately weighed weight, then, cooling, weighing 1 hour dry in above-mentioned temperature, until
Until the difference weighed twice in succession is no more than 5mg.According to the weight of less loss, water content (%) in test sample is calculated.As a result see
Table 2.
The imperial sample moisture measurement result of 2 grass of table
The result shows that 11 batches of sample moisture contents are between 9.0~12.6%, it is averagely aqueous to be divided into 10.4%.Therefore it drafts
This product standard aqueous point must not exceed 15.0%.
Total ash measurement: referring to (the 1. total ashes measurement of one annex of " Chinese Pharmacopoeia " version in 2010, Ⅸ K Ash determination method
Method) 11 batches of samples progress total ashes are measured.The imperial medicinal material of different sources grass (crossing No. 2 sieves) about 4.0g is taken, according to " middle traditional Chinese medicines
Allusion quotation " total ash measuring method (Ⅸ K of annex) measures under 2010 years one Ash determination method items of version.The sample of measurement must crush, and make
2~3g of sample (such as palpus measurement acid-insoluble ash, can use for 3~5g of sample) can be taken, is set by No. two sieves, after mixing
In the crucible of ignition to constant weight, weighed weight (accurately to 0.01) is slowly scorching hot, pays attention to avoiding burning, until when carbonizing completely, 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
(%).It the results are shown in Table 3.
The imperial sample total ash measurement result of 3 grass of table
The result shows that 11 batches of sample total ashes are 4.4%~12.7%, average total ash content is 7.8%.Therefore quasi- regulation
This product standard total ash must not cross 13.0%.
Acid insoluble ash: referring to one annex of " Chinese Pharmacopoeia " version in 2010, Ⅸ K Ash determination method, (2. acid insoluble ash are surveyed
Determine method) 11 batches of samples are measured.According to acid-insoluble ash under one Ash determination method item of " Chinese Pharmacopoeia " version in 2010
Measuring method (Ⅸ K of annex) measurement.The resulting ash content of item is taken, pays attention to that dilute hydrochloric acid about 10ml is added in crucible, is covered with surface plate
Lid crucible is set and is heated 10 minutes in water-bath, and surface plate is rinsed with hot water 5ml, and washing lotion is incorporated in crucible, is filtered with ashless filter paper,
Residue in crucible is washed with water on filter paper, and washs until the not aobvious chloride reaction of washing lotion.Filtrate moves to together together with filter paper
It is dry in one crucible, ignition to constant weight.According to residue weight, acid-insoluble ash weight (%) in test sample is calculated.As a result see
Table 4.
The imperial sample acid-insoluble ash measurement result of 4 grass of table
According to said determination as a result, 11 batches of sample acid-insoluble ash contents are between 0.1%~1.5%, average acid is not
Dissolubility content of ashes is 0.6%.Therefore quasi- regulation this product standard acid-insoluble ash must not exceed 2.0%.
Extract is according to the one hot dipping measurement of " Chinese Pharmacopoeia " version in 2010.Test sample about 2~4g is taken, it is accurately weighed,
It sets in the conical flask of 100~250ml, precision plus 50~100ml of water, close plug, weighed weight, after standing 1 hour, connects returned cold
Solidifying pipe, is heated to boiling, and kept for slightly boiled 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, is supplied and is subtracted with water
The weight of mistake, shakes up, and is filtered with drier, and precision measures filtrate 25ml, sets and has dried into the evaporating dish of constant weight, in water-bath
It is 3 hours dry in 105 DEG C after being evaporated, set 30 minutes cooling in drier, rapid accurately weighed weight.Unless otherwise specified, with
Dry product calculates the content (%) of water-soluble extractives in test sample.It the results are shown in Table 5.
The imperial sample determination of extractives result of 5 grass of table
According to said determination as a result, 11 batches of sample extracts are between 10.3%~34.2%, average extract is
21.6%.In view of the difference of crude drug source, therefore drafts this product standard extract content and be no less than 10.0%.
5 assay of embodiment
One, instrument and material
LC-20AT high performance liquid chromatograph (band autosampler) diode array detector, LCsolution chromatography work
It stands (being Japanese Shimadzu Corporation)；KQ-100.DE type numerical control ultrasonic cleaner (Kunming Ultrasound Instrument Co., Ltd)；
X205BDU electronic analytical balance (Mei Tele company, Switzerland)；EASY PURE II Superpure water machine (power & light company, the U.S.) etc..Do not eat
Son acid reference substance (Chengdu Man Site Biotechnology Co., Ltd, content: 98%, lot number: MUST-13040103)；Mobile phase institute
With methanol be chromatographically pure (Fisher company, the U.S.), water is ultrapure water, remaining is that analysis is pure.
Two, method
Using octadecylsilane chemically bonded silica as filler, chromatographic column is Gemini C18(4.6mm × 250mm, 5 μm)；With
- 0.1% phosphoric acid of methanol (1:99) is mobile phase；25 DEG C of column temperature, Detection wavelength 272nm.Number of theoretical plate is based on gallic acid peak
2000 should be not less than by calculating.Precision claims gallic acid reference substance appropriate, adds water that the solution of every 1ml 30 μ g containing gallic acid is made, i.e.,
Obtain reference substance solution.This product powder (crossing No. four sieves) 0.2g is taken, it is accurately weighed, it sets in tool plug round-bottomed flask, precision is added 10%
Hydrochloric acid solution 25ml, weighed weight set and are heated to reflux 30mim in water-bath, lets cool, then weighed weight, are supplied and are subtracted with 10% hydrochloric acid
The weight of mistake, shakes up, and filtering takes subsequent filtrate up to test solution.It is accurate respectively to draw reference substance solution and test solution
Each 10 μ l, inject liquid chromatograph, measurement to get.
As a result: on test solution and the photograph corresponding position of product solution chromatogram, time of withing a hook at the end identical chromatographic peak, and
Negative controls chromatogram is then without this chromatographic peak.See Fig. 6.
1 > linear relationship is investigated
It takes gallic acid reference substance appropriate, adds water that the solution of 0.5mg/ml is made, it is accurate respectively to draw 0.2,1,2,3,4,
5ml, respectively plus water is settled to 5ml, shakes up.It is accurate respectively to draw above-mentioned each 10 μ l of test solution, HPLC is injected, with gallic acid
Peak area is ordinate, and sample volume (μ g) is abscissa, draws standard curve.Obtain the regression equation of gallic acid: Y=
2770704.84x-89286, r=0.9999, gallic acid are in good line with peak area in 0.1974~4.935 μ g range
Sexual intercourse.
2 > precision test
Same test solution is taken, is measured 5 times by above-mentioned chromatographic condition continuous sample introduction.As a result: 5 measurement gallic acid peaks
The RSD=0.54% of area.Show that instrument precision is good.
3 > repetitive test
6 parts of same sample powder are taken, every part of 0.2g is accurately weighed, prepares test solution, surveys by above-mentioned chromatographic condition
It is fixed.As a result: the RSD of gallic acid content is 1.30% in 6 parts of test solutions.Show that this method reproducibility is good.
4 > stability test
Same test solution is taken, by above-mentioned chromatographic condition, respectively at 1,2,4,8,12, sample introduction is measured for 24 hours.As a result: sample
The RSD of gallic acid peak area is 0.85% in product.Show that the gallic acid in test solution is good in internal stability for 24 hours
It is good.
The test of 5 > sample recovery rate
Oneself is taken to know 6 parts, each 0.1g of content same sample powder, accurately weighed, gallic acid reference substance solution is added in precision
(68 μ g/ml) 25ml, prepares test solution, by above-mentioned chromatographic condition measure gallic acid content, calculate average recovery rate and
RSD.As a result: measurement gallic acid content average recovery rate is 97.54%, RSD=1.99%.
Three, sample measures
Referring to " Chinese Pharmacopoeia " 2010 editions annex VI D high performance liquid chromatographies, according to the method described above to 11 batch medicines
Material sample is measured, and the results are shown in Table 6.
6 sample size measurement result (n=2) of table
The result shows that: 11 batches of sample gallic acid contents are 0.69%~5.14%, average content 2.61%.According to 11
Criticize the measurement result of sample, it is contemplated that crude drug source difference condition is drafted this product standard and calculated by dry product containing gallic acid
(C7H6O5) 0.50% must not be less than.
Claims (3)
1. a kind of quality determining method of the imperial medicinal material of grass, it is characterised in that mainly include Medicinal Materials Characters identification, microscopical characters, thin layer
Identification and assay,
During the Medicinal Materials Characters identify, medicinal material root is cylindrical, and lark is slightly bent, pogoniasis root, 0.3~0.8cm of diameter；Stem
Surface celadon has thin vertical wrinkle, is in Dark grey at excoriation, matter is soft, frangibility, and section skin zone is thin, yellowish-white to taupe
There is wide marrow at color, woody part ivory buff, center；Leaf papery, lanceolar, more shrinkages, full edge have dilute pubescence, upper surface ash
Green, lower surface taupe, long 8~13cm, wide 2~5cm；Gas is micro-, bitter；Moisture must not exceed 15.0% in medicinal material, total ash
Divide and must not exceed 13.0%, acid-insoluble ash must not exceed 2.0%, and water-soluble extractives must not be lower than 10.0%；
In the microscopical characters, medicinal powder is in yellow-white, and needle-like calcium oxalate crystal and cluster crystal are common, and needle is 28~71 μm long, 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 12~184 μm long；
The thin layer, which identifies, uses silica gel H lamellae, using toluene-ethyl acetate-acetone-formic acid solution as solvent, with 1%
- 1% liquor ferri trichloridi mixed solution of potassium ferricyanide solution is color developing agent；Thin layer identifies to be carried out by following operation: taking test sample
5 μ l of solution, 5 μ l of reference substance solution are put respectively on same silica gel H lamellae, with toluene-second of volume ratio 5:4:0.5:0.5
Acetoacetic ester-acetone-formic acid solution is unfolded as solvent, takes out, dries；It sprays molten with 1% potassium ferricyanide of volume ratio 1:1
The mixed solution of -1% liquor ferri trichloridi of liquid, daylight are inspected；
The assay is carried out by following operation: using octadecylsilane chemically bonded silica as filler；With volume ratio 1:99's
- 0.1% phosphoric acid mixed solution of methanol is mobile phase；25 DEG C of column temperature, Detection wavelength 272nm；Number of theoretical plate presses gallic acid peak
2000 should be not less than by calculating；It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is surveyed
It is fixed to get.
2. the quality determining method of the imperial medicinal material of grass according to claim 1, it is characterised in that the confession in the thin layer identification
Test product and reference substance press following operation preparation: using solution made of careless imperial herb medicinal powder as test sample, taking medicinal powder
0.5g adds water 20ml, is ultrasonically treated 30 minutes, and filtration, filtrate is evaporated, and methanol constant volume is added to 1ml, as test solution；
Gallic acid reference substance separately is taken, adds methanol that the solution of every ml 1mg containing gallic acid is made.
3. the quality determining method of the imperial medicinal material of grass according to claim 1, it is characterised in that the confession in the assay
Test product and reference substance press following operation preparation: precision claims gallic acid reference substance appropriate, adds water that every 1ml is made containing gallic acid 30
The solution of μ g is to get reference substance solution；Medicinal powder 0.2g is taken, it is accurately weighed, it sets in tool plug round-bottomed flask, precision is added 10%
Hydrochloric acid solution 25ml, weighed weight set and are heated to reflux 30mim in water-bath, lets cool, then weighed weight, are supplied and are subtracted with 10% hydrochloric acid
The weight of mistake, shakes up, and filtering takes subsequent filtrate to get test solution.
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| CN1971272A (en) * | 2006-11-30 | 2007-05-30 | 贵州益佰制药股份有限公司 | Quality control method of beautyberry grass-blade |
| CN101477102A (en) * | 2008-12-10 | 2009-07-08 | 上海康桥中药饮片有限公司 | Quality standard of south yew decoction pieces and its detection method |
| CN104374862A (en) * | 2014-11-27 | 2015-02-25 | 成都大学 | Salvia miltiorrhiza stem leaf quality control method |
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| CN1971272A (en) * | 2006-11-30 | 2007-05-30 | 贵州益佰制药股份有限公司 | Quality control method of beautyberry grass-blade |
| CN101477102A (en) * | 2008-12-10 | 2009-07-08 | 上海康桥中药饮片有限公司 | Quality standard of south yew decoction pieces and its detection method |
| CN104374862A (en) * | 2014-11-27 | 2015-02-25 | 成都大学 | Salvia miltiorrhiza stem leaf quality control method |
Non-Patent Citations (3)
| Title |
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| 民族药草龙药材的质量控制研究;李兵 等;《安徽农业科学》;20121231;第40卷(第27期);13338-13339 |
| 草龙化学成分的研究;卢汝梅 等;《中草药》;20090930;第40卷(第9期);1372-1374页 |
| 高效液相色谱法测定草龙中没食子酸的含量;周小雅 等;《西北药学杂志》;20140531;第29卷(第3期);235-237页 |
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