CN110376316A - The method of quality control of Calusena lansium root herb - Google Patents
The method of quality control of Calusena lansium root herb Download PDFInfo
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Abstract
The invention discloses a kind of method of quality control of Calusena lansium root herb, mainly include Imperatorin assay, and assay uses methanol ultrasonic extraction Calusena lansium root herb, using methanol-water as mobile phase, Detection wavelength 300nm.Experiment shows that the method has stronger specificity and good reproducibility.Accordingly, the thin layer that inventor further studies Calusena lansium root herb identifies, character identifies (moisture content, ash content and extract) and microscopical characters, provides scientific basis to work out scientific, complete, reliable, effective Chinese wampee root quality of medicinal material standard.To sum up, the present invention can be used for thoroughly evaluating Chinese wampee root quality of medicinal material, and Chinese wampee root quality of medicinal material can be effectively controlled, it is ensured that the medicinal material uses safe and effective.
Description
Technical field
The invention belongs to Chinese herbal medicine quality of medicinal material control technology fields more particularly to a kind of quality of Calusena lansium root herb to control
Method.
Background technique
Chinese wampee root is the dry root of rutaceae Calusena lansium Clausena lansium (Lour.) Skeels.Calusena lansium, also known as
Golden bullet, yellow bullet, yellow wingceltis etc., in " Chinese Plants will ", " China's book on Chinese herbal medicine ", " national Chinese herbal medicine compilation ", " Chinese Higher plant figure
Mirror ", " guangxi plant will " " guangxi plant register ", " Medicinal Plants of Guangxi register ", " strong medicine a collection of selected materials ", " Chinese precious jade pharmacy " etc. write
Oppose its former plant, geographical distribution, Medicinal or medical value etc. also has description.Through consult go through version " Chinese Pharmacopoeia " and " extensively
Western Chinese medicine standard " etc. each place standard, do not have recording for Chinese wampee root quality standard.Chinese wampee root is one and multi-national uses
Traditional herbal medicine has use in the civil of ground such as the Guangxi, Fujian, Jiangxi in China.It is used as medicine in the civil Calusena lansium of Guangxi Zhuang precious jade with root
When, bitter, peppery, slightly warm in nature have clearing damp poison, remove miasm, and the function of dispersing wind and cold is used for energy-stagnation stomachache, abdominal pain, colic, rheumatic bone
Bitterly, dysmenorrhea, jaundice, malaria, prevention stream.Calusena lansium original plant China be distributed mainly on Taiwan, Fujian, Guangxi, Guangdong, Hainan,
The ground such as Guizhou, Yunnan, Sichuan.There are cultivation in Guangxi whole district various regions.Calusena lansium is mostly cultivation product, is born in loose, fertile, wet soil
Earth.
Calusena lansium is entered with positions such as root, leaf, fruit, fruit stones medicinal civil, and Guangxi Zhuang precious jade is civil to be mostly used as medicine with its root, it is annual
It can harvest, cleaning, drying.Chinese wampee root Imperatorin containing furoeoumarin, Calusena lansium furoeoumarin (i.e. dehydrogenation print Calusena lansium lactone),
8- Mang ox oxygroup psoralen, sequiterpene ketone dextrorotation Apostichopus japonicus terpene ketone, kappa azoles alkaloid 3- formoxyl -6- methoxyl group card
Bar azoles, 6- methoxyl group kappa azoles -3- carboxylate methyl ester, 3- formoxyl -1,6- dimethoxy kappa azoles, 3- formoxyl kappa azoles, card
Bar azoles -3- carboxylate methyl ester, murrayanine, glycozoline, India's Calusena lansium azoles alkali etc..Document report, Imperatorin contained by Chinese wampee root
There is apoptotic effect to growth cell with cytotoxicity, and only, acts on the G1/S transition phase in the cell cycle, which has
Potential development becomes the drug for having selective toxicity to tumour cell.Pharmacological evaluation proves that Imperatorin, which has, inhibits epilepsy
Breaking-out, expansion blood vessel inhibit myocardial hypertrophy, inhibition tumor cell proliferation, antimicrobial, the metabolic enzymatic activity of influence etc. a variety of
Pharmacological action.Document report clinically has doctor to be shared with lantern bubble grass, Chinese wampee root over several years and cured more than 20 example of orchitis, curative effect
It is satisfied；Or treated and had a stomachache with Chinese wampee root, effectively.
Chinese wampee root has been approved in civil clinical efficacy effect, but as the civil medicinal herbs most in use of Guangxi Zhuang precious jade, Calusena lansium
Root does not establish method of quality control, it is difficult to control medical material quanlity, be unfavorable for production, circulation, use, the inspection of Calusena lansium root herb
It tests, manage.Therefore, it is necessary to establish the method for quality control of Chinese wampee root, to control the quality of Calusena lansium root herb.Currently, there is not yet
To the report of the correlative studys such as character identification, microscopical characters, thin layer identification, assay about Calusena lansium root herb.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of quality of scientific, complete, reliable, effective Calusena lansium root herb
Control method.
In order to solve the above technical problems, the invention adopts the following technical scheme:
The method of quality control of Calusena lansium root herb, mainly includes Imperatorin assay, and assay is super using methanol
Sound extracts Calusena lansium root herb, using methanol-water as mobile phase, Detection wavelength 300nm.
Assay is carried out by following operation: using octadecylsilane chemically bonded silica as filler；With volume ratio 55:45's
Methanol-water is mobile phase；25 DEG C of column temperature, Detection wavelength 300nm；It is accurate respectively to draw reference substance solution and test solution each 10
μ l, inject liquid chromatograph, measurement to get.
Reference substance solution presses following operation preparation: precision claims Imperatorin reference substance appropriate, adds methanol that every 1ml is made containing Europe
The solution of 30 μ g of peucedanin to get；Test solution is by following operation preparation: taking Chinese wampee root medicinal powder (crossing No. four sieves)
0.5g, it is accurately weighed, it sets in conical flask, methanol 15ml, close plug, weighed weight, ultrasonic treatment (power 150W, frequency is added in precision
Rate 40KHZ) 30 minutes, let cool, then weighed weight, the weight of less loss supplied with methanol, is shaken up, filter, take subsequent filtrate to get.
The method of quality control of above-mentioned Calusena lansium root herb further includes that thin layer identifies, and thin layer, which identifies, uses silica gel g thin-layer plate,
Using dimethylbenzene-ethyl acetate solution as solvent.
Thin layer identifies to be carried out by following operation: drawing test solution, control medicinal material solution each 3 μ l, 1 μ of reference substance solution
L is put respectively on same silica gel g thin-layer plate, is opened up using dimethylbenzene-ethyl acetate solution of volume ratio 10:1.5 as solvent
It opens, takes out, dry, set and inspected under ultraviolet lamp (365nm).
Test solution or control medicinal material solution are by following operation preparation: taking Chinese wampee root medicinal powder or Chinese wampee root comparison medicine
Material powder 1g, adds ethyl alcohol 10ml, is ultrasonically treated 30 minutes, and filtration, filtrate is evaporated, residue add ethyl alcohol 1ml make dissolution to get；It is right
According to product solution by following operation preparation: taking Imperatorin reference substance, add ethyl alcohol that the solution of every ml 1mg containing Imperatorin is made.
The method of quality control of above-mentioned Calusena lansium root herb further includes that Medicinal Materials Characters identify, and in character identification, medicinal material is not advise
Then oval column or coniform, slightly curved song, varying length, 0.5~6.0cm of diameter or wider；Surface taupe brown is to deep yellow palm fibre
Color, it is coarse, have thin vertical wrinkle and radicula trace；Cork is easy to fall off, and the place that falls off is in sundown；Matter is hard, is not easily broken, section skin
Portion and woody part boundary line are obvious, skin zone's light brown, and woody part is faint yellow, it is seen that proper alignment ring grain；Gas is micro-, puckery.
The method of quality control of above-mentioned Calusena lansium root herb, further includes medicinal material microscopical characters, in microscopical characters, root cross section
Phellem layer is that ordered series of numbers square circular or polygonal cell, some fall off；Cortical cell square circular or irregular shape, cell size is not
One；Phloem cell similar round, some shrinkage deformations, the several annular distributions interrupted in groups of bast fiber, with phloem parenchyma cell
Between layered arrangement, form brilliant sheath fiber containing calcium oxalate prismatic crystal in the parenchyma cell of fiber peripheral；Xylem is broad, and conduit is single
Or several gatherings are dispersed in distribution, 36~98 μm of diameter, ray cell 1~2 arranges；Cell similar round in the middle part of root, wall thickness, woodization；Skin
The starch-containing grain and calcium oxalate prismatic crystal having in the parenchyma cell of layer and bast；Medicinal powder is in faint yellow；Wood-fibred bunchy or
Separation, slightly bent, apex is tapering, round blunt or fractures, and fibre wall is relatively thin, and cell is larger, there is dotted or linear type pit, diameter 13
~25 μm；The more bunchys of bast fiber, yellow green form brilliant sheath fiber containing calcium oxalate prismatic crystal in the parenchyma cell of fiber peripheral,
16~26 μm of diameter；Calcium oxalate prismatic crystal shape is different, and 8~25 μm of diameter；Amylum body is composite grain or simple grain, and omphalion is dotted, simple grain
3~8 μm of diameter；Conduit is bordered pit vessel, 31~52 μm of diameter；Cork cell's polygonal or similar round, brown color.
Aiming at the problem that current Calusena lansium root herb lacks related quality criterion, inventor is on the basis of prior art means
On, by the research of scientific system, a kind of method of quality control of Calusena lansium root herb is established, mainly includes Imperatorin content
Measurement, assay use methanol ultrasonic extraction Calusena lansium root herb, using methanol-water as mobile phase, Detection wavelength 300nm.It is real
It tests and shows that the method has stronger specificity and good reproducibility.Accordingly, inventor further studies Calusena lansium root herb
Thin layer identifies, character identifies (moisture content, ash content and extract) and microscopical characters, scientific, complete, reliable, effective to work out
Chinese wampee root quality of medicinal material standard provides scientific basis.To sum up, the present invention can be used for thoroughly evaluating Chinese wampee root quality of medicinal material, effectively
The product quality of guarantee and specification Calusena lansium root herb, it is ensured that people's drug safety.
Detailed description of the invention
Fig. 1 is the structural map in Chinese wampee root cross section, and in figure: 1 phellem layer, 2 cortexes, 3 bast fibers, 4 basts, 5 is wooden
Portion, 6 conduits.
Fig. 2 is the structural map of Chinese wampee root powder, in figure: 1 amylum body, 2 calcium oxalate cluster crystals, 3 cork cells, 4 wood-fibreds, 5
Bast fiber, 6 conduits.
Fig. 3 is the thin layer identification figure of 11 kinds of different sources Chinese wampee roots, and in figure: 1-11 is 1#~11# different sources respectively
Calusena lansium root herb, 4# are Chinese wampee root control medicinal materials；12. Imperatorin reference substance；A, B, C, D, E are yellow green spot.
Fig. 4 is that HPLC schemes, in figure: A reference substance, B test sample, C negative control.
Specific embodiment
Calusena lansium root herb used in following example comes from 11 different sources, is accredited as rutaceae Calusena lansium through pharmacist
The dry root of Clausena lansium (Lour.) Skeels.Crude drug source details are shown in Table 1.
1 different sources Chinese wampee root of table number
1 character of embodiment identifies
The character of Calusena lansium root herb from 11 different sources is identified, as the result is shown: Calusena lansium root herb is not
The oval column or coniform of rule, slightly curved song, varying length, 0.5~6.0cm of diameter or wider.Surface taupe brown is to deep yellow palm fibre
Color, it is coarse, have thin vertical wrinkle and radicula trace.Cork is easy to fall off, and the place that falls off is in sundown.Matter is hard, is not easily broken, section skin
Portion and woody part boundary line are obvious, skin zone's light brown, and woody part is faint yellow, it is seen that proper alignment ring grain.Gas is micro-, puckery.
2 microscopical characters of embodiment (Fig. 1, Fig. 2)
The microstructure of Calusena lansium root herb from 11 different sources is identified, as the result is shown: (Fig. 1) Chinese wampee root
Root cross section phellem layer be that ordered series of numbers square circular or polygonal cell, some fall off.Cortical cell square circular or irregular shape, carefully
Born of the same parents are not of uniform size.Phloem cell similar round, some shrinkage deformations, the several annular distributions interrupted in groups of bast fiber, with bast
Layered arrangement between parenchyma cell forms brilliant sheath fiber containing calcium oxalate prismatic crystal in the parenchyma cell of fiber peripheral.Xylem is broad,
Conduit is single or several meet is dispersed in distribution, and 36~98 μm of diameter, ray cell 1~2 arranges；Cell similar round in the middle part of root, wall thickness,
Woodization.The starch-containing grain and calcium oxalate prismatic crystal having in the parenchyma cell of cortex and phloem.
In addition, inventor has also carried out microexamination to all Chinese wampee root medicinal powders, as a result as follows: (Fig. 2) powder is in
It is faint yellow.Wood-fibred bunchy or separation, slightly bent, apex is tapering, round blunt or fractures, and fibre wall is relatively thin, and cell is larger, has dotted
Or linear type pit, 13~25 μm of diameter；The more bunchys of bast fiber, yellow green contain oxalic acid in the parenchyma cell of fiber peripheral
Calcium prismatic crystal forms brilliant sheath fiber, and 16~26 μm of diameter.Calcium oxalate prismatic crystal shape is different, and 8~25 μm of diameter.Amylum body be composite grain or
Simple grain, omphalion is dotted, and 3~8 μm of simple grain diameter.Conduit is bordered pit vessel, 31~52 μm of diameter.Cork cell's polygonal or
Similar round, brown color.
To sum up, the microscopical characters main points of Calusena lansium root herb are as follows: the several annular distributions interrupted in groups of root cross section bast fiber；
Visible bordered pit vessel in powder；Cross section and the visible calcium oxalate prismatic crystal of powder and amylum body.
3 thin-layer chromatographic analysis of embodiment
Using solution made of Chinese wampee root medicinal powder as test sample, medicinal material powder 1g is taken, adds ethyl alcohol 10ml, ultrasonic treatment 30
Minute, filtration, filtrate is evaporated, and residue adds ethyl alcohol 1ml to make to dissolve, as test solution；Chinese wampee root control medicinal material 1g separately is taken, together
Control medicinal material solution is made in method；Imperatorin reference substance is taken again, adds ethyl alcohol that solution of every 1ml containing 1mg is made, it is molten as reference substance
Liquid.It is tested according to thin-layered chromatography (Chinese Pharmacopoeia version general rule 0502 in 2015), draws test solution, each 3 μ of control medicinal material solution
L, 1 μ l of reference substance solution are put respectively on same silica gel g thin-layer plate, with dimethylbenzene-ethyl acetate (10:1.5) for solvent,
Expansion takes out, dries, set and inspect under ultraviolet lamp (365nm).
Measure 11 batches of medicinal material samples, as a result as shown in figure 3, in sample chromatogram, with reference medicine chromatography and reference substance
On the corresponding position of chromatography, 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
Different sources Chinese wampee root medicinal powder is taken, according under " Chinese Pharmacopoeia " 0832 aquametry item of version general rule in 2015
Second method (oven drying method) measurement.2~5g of test sample is taken, is laid in drying into the flat weighing bottle of constant weight, thickness is no more than 5mm,
Loose test sample is no more than 10mm, accurately weighed, and unlatching bottle cap is 5 hours dry at 100~105 DEG C, and bottle cap is covered, is moved to dry
It in dry device, lets cool 30 minutes, accurately weighed then 1 hour dry in above-mentioned temperature, cooling, weighing, until the difference weighed twice in succession
It is different be no more than 5mg until.According to the weight of less loss, water content (%) in test sample is calculated.It the results are shown in Table 2.
2 Chinese wampee root sample moisture measurement result of table
The result shows that 11 batches of sample moisture contents are between 9.8~10.0%, it is averagely aqueous to be divided into 8.5%.Therefore draft this
Product standard aqueous point must not exceed 12.0%.
Total ash measurement: right referring to " Chinese Pharmacopoeia " 2015 2302 Ash determination method of version general rule (1. total ash measuring method)
11 batches of samples carry out total ash and are measured.Different sources Calusena lansium root herb is taken, according to " Chinese Pharmacopoeia " version general rule in 2015
Total ash measuring method measurement under 2302 Ash determination method items.The test sample of measurement must crush, and enable through No. two sieves, mixing
After uniformly, 2~3g of sample (as acid-insoluble ash must be measured, can use for 3~5g of sample) is taken, the crucible of ignition to constant weight is set
In, weighed weight (it is slowly red-hot accurately to 0.01g), pay attention to avoiding burning, until completely charing when, gradually rise temperature to 500
~600 DEG C, make to be ashed completely and to constant weight.According to residue weight, the content (%) of total ash in test sample is calculated.It the results are shown in Table 3.
3 Chinese wampee root sample total ash measurement result of table
The result shows that 11 batches of sample total ashes are 1.3%~2.6%, average total ash content is 2.0%.Therefore quasi- regulation
This product standard total ash must not cross 5.0%.
Acid insoluble ash: referring to " Chinese Pharmacopoeia " 2302 Ash determination method of version general rule (2. acid insoluble ash measurement in 2015
Method) 11 batches of samples are measured.By acid-insoluble ash under " Chinese Pharmacopoeia " 2302 Ash determination method item of version general rule in 2015
Measuring method measurement.The resulting ash content of item is taken, dilute hydrochloric acid about 10ml is carefully added into crucible, crucible is covered with surface plate, sets
It is heated 10 minutes in water-bath, surface plate is rinsed with hot water 5ml, and washing lotion is incorporated in crucible, is filtered with ashless filter paper, residual in crucible
Slag is washed with water on filter paper, and washs until the not aobvious chloride reaction of washing lotion.Filtrate moves in same crucible together with filter paper, does
It is dry, ignition to constant weight.According to residue weight, the content (%) of acid-insoluble ash in test sample is calculated.It the results are shown in Table 4.
4 Chinese wampee root sample acid-insoluble ash measurement result of table
According to said determination as a result, 11 batches of sample acid-insoluble ash contents are between 0.1%~0.5%, average acid is not
Dissolubility content of ashes is 0.2%.Therefore quasi- regulation this product standard acid-insoluble ash must not exceed 2.0%.
Extract: referring to " Chinese Pharmacopoeia " 2201 Extract mensuration of version general rule (2. ethanol soluble extractives measurement in 2015
Method) 11 batches of samples are measured.According to the alcohol-soluble leaching under " Chinese Pharmacopoeia " 2201 Extract mensuration item of version general rule in 2015
Object measuring method out is measured using hot dipping.Test sample about 2~4g is taken, it is accurately weighed, it sets in the conical flask of 100~250ml, essence
Close plus 50~100ml of Diluted Alcohol, close plug, weighed weight after standing 1 hour, connect reflux condensing tube, are heated to boiling, and protect
It holds slightly boiled 1 hour.After letting cool, conical flask, close plug, then weighed weight are removed, the weight of less loss is supplied with Diluted Alcohol, is shaken up, used
Dry filter filtration, precision measure filtrate 25ml, set and dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C
It is 3 hours dry, set 30 minutes cooling in drier, rapid accurately weighed weight.Unless otherwise specified, it is calculated with dry product for examination
The content (%) of ethanol soluble extractives in product.It the results are shown in Table 5.
5 Chinese wampee root sample determination of extractives result of table
According to said determination as a result, between 11 batches of sample extracts 2.3%~10.2%, average extract is 5.8%.It examines
Consider the difference of crude drug source, therefore drafts this product standard extract content and be no less than 2.0%.
5 assay of embodiment
One, instrument and material
1260 type high performance liquid chromatographs (agilent company, band autosampler and VWD detector)；KQ-3200DE type
Numerical control ultrasonic cleaner (Kunming ultrasonic instrument Co., Ltd)；Ten a ten thousandth electronic analytical balance (Switzerland Mei Te of XS205
Le-support benefit company)；II Superpure water machine of EASYPURE (power & light company, the U.S.) etc..Imperatorin reference substance (Chinese food drug
Examine and determine research institute, lot number 110826-201415, purity 99.7%, for assay)；Methanol, acetonitrile used in mobile phase is
Chromatographically pure (German merck company), water are ultrapure water, remaining reagent is that analysis is pure.
Two, method
Using octadecylsilane chemically bonded silica as filler, chromatographic column is Féraud door Gemini NX-C18(4.6mm×
250mm, 5 μm)；With methanol-water (55:45) for mobile phase；25 DEG C of column temperature, Detection wavelength 300nm.Number of theoretical plate presses Imperatoria ostruthium
Plain peak, which calculates, should be not less than 3000.Precision claims Imperatorin reference substance appropriate, and methanol is added to be made every 1ml 30 μ g's containing Imperatorin
Solution is to get reference substance solution.Chinese wampee root medicinal powder (crossing No. four sieves) about 0.5g is taken, it is accurately weighed, it sets in conical flask, it is accurate
Methanol 15ml, close plug is added, weighed weight is ultrasonically treated (power 150W, frequency 40KHZ) 30 minutes, lets cool, then weighed heavy
Amount, the weight of less loss is supplied with methanol, is shaken up, and is filtered, is taken subsequent filtrate to get test solution.It is accurate respectively to draw reference substance
Solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.
As a result: as shown in figure 4, the time of withing a hook at the end is identical on test solution and the photograph corresponding position of product solution chromatogram
Chromatographic peak, and negative controls chromatogram is then without this chromatographic peak.
1 > linear relationship is investigated
It takes Imperatorin reference substance appropriate, adds methanol that the solution of 0.328mg/ml is made, it is accurate respectively to draw 0.2,1,2,
3,4,5ml, respectively plus methanol constant volume is to 10ml, shakes up.It is accurate respectively to draw above-mentioned each 10 μ l of test solution, HPLC is injected, with
Imperatorin peak area is ordinate, and sample volume (μ g) is abscissa, draws standard curve.Obtain the recurrence side of Imperatorin
Journey: Y=2400.3X+3.0694, r=0.9998, Imperatorin reference substance sample volume in 0.0656~1.6400 μ g range with
Peak area is in good linear relationship.
2 > precision test
Same test solution is taken, is measured 6 times by above-mentioned chromatographic condition continuous sample introduction.As a result: 6 measurement Imperatorin peaks
The RSD=0.59% of area.Show that instrument precision is good.
3 > repetitive test
6 parts of same sample powder are taken, every part of 0.5g is accurately weighed, prepares test solution, surveys by above-mentioned chromatographic condition
It is fixed.As a result: the RSD of 6 parts of test solution Determination of Imperatorin is 0.96%.Show that this method reproducibility is good.
4 > stability test
Same test solution is taken, by above-mentioned chromatographic condition, respectively at 0,2,4,6,12, sample introduction measurement for 24 hours.As a result: 6 times
The Imperatorin content RSD measured is 0.87%.Show that Imperatorin in test solution has good stability within for 24 hours.
The test of 5 > sample recovery rate
Oneself is taken to know 6 parts, each 0.25g of content same sample powder, accurately weighed, Imperatorin reference substance solution is added in precision
(26.61 μ g/ml) 15ml, prepares test solution, measures Imperatorin content by above-mentioned chromatographic condition, calculates average recovery rate
And RSD.As a result: measurement Imperatorin content average recovery rate is 97.2%, RSD=0.89%.
Three, sample measures
Referring to " Chinese Pharmacopoeia " 2015 editions 0512 high performance liquid chromatographies of general rule, 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 Imperatorin contents are 0.04%~0.36%, average content 0.16%.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 Imperatorin
(C16H14O4) 0.04% must not be less than.
Claims (8)
1. a kind of method of quality control of Calusena lansium root herb, it is characterised in that mainly include Imperatorin assay, containing measurement
Surely methanol ultrasonic extraction Calusena lansium root herb, using methanol-water as mobile phase, Detection wavelength 300nm are used.
2. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that the assay press with
Lower operation carries out: using octadecylsilane chemically bonded silica as filler；Using the methanol-water of volume ratio 55:45 as mobile phase；Column temperature
25 DEG C, Detection wavelength 300nm；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.
3. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that: the reference substance solution is pressed
Following operation preparation: precision claim Imperatorin reference substance, add methanol be made the solution of every 1ml 30 μ g containing Imperatorin to get；Institute
Test solution is stated by following operation preparation: taking Chinese wampee root medicinal powder 0.5g, it is accurately weighed, it sets in conical flask, precision is added
Methanol 15ml, close plug, weighed weight, ultrasonic treatment, power 150W, frequency 40KHZ 30 minutes, are let cool, then weighed weight, are used
Methanol supplies the weight of less loss, shakes up, filtration, take subsequent filtrate to get.
4. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that it further include that thin layer identifies, it is thin
Layer, which identifies, uses silica gel g thin-layer plate, using dimethylbenzene-ethyl acetate solution as solvent.
5. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that the thin layer identify by with
Lower operation carries out: drawing test solution, each 3 μ l of control medicinal material solution, 1 μ l of reference substance solution is put thin in same silica G respectively
On laminate, it is unfolded using dimethylbenzene-ethyl acetate solution of volume ratio 10:1.5 as solvent, takes out, dry, set ultraviolet light
It is inspected under lamp 365nm.
6. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that: the test solution or
Control medicinal material solution is by following operation preparation: Chinese wampee root medicinal powder or Chinese wampee root control medicinal material powder 1g taken, ethyl alcohol 10ml is added,
Ultrasonic treatment 30 minutes, filtration, filtrate is evaporated, residue add ethyl alcohol 1ml make dissolution to get；The reference substance solution presses following behaviour
It prepares: taking Imperatorin reference substance, add ethyl alcohol that the solution of every ml 1mg containing Imperatorin is made.
7. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that further include Medicinal Materials Characters mirror
Not, during the character identifies, medicinal material is irregular oval column or coniform；Surface taupe brown is to deep yellow brown, and coarse, tool is thin
Vertical wrinkle and radicula trace；Cork is easy to fall off, and the place that falls off is in sundown；Matter is hard, is not easily broken, section skin zone and woody part boundary line
Obviously, skin zone's light brown, woody part is faint yellow, sees proper alignment ring grain；Gas is micro-, puckery.
8. the method for quality control of Calusena lansium root herb according to claim 1, it is characterised in that further include the micro- mirror of medicinal material
Not, in the microscopical characters, the phellem layer in root cross section is ordered series of numbers square circular or polygonal cell；Cortical cell square circular or not
Regular shape；Phloem cell similar round, the several annular distributions interrupted in groups of bast fiber, stratiform is arranged between phloem parenchyma cell
It arranges, forms brilliant sheath fiber containing calcium oxalate prismatic crystal in the parenchyma cell of fiber peripheral；Xylem is broad, and conduit is single or several phases
Poly- to be dispersed in distribution, 36~98 μm of diameter, ray cell 1~2 arranges；Cell similar round in the middle part of root, wall thickness, woodization；Medicinal powder is in
It is faint yellow；Wood-fibred bunchy or separation, apex is tapering, round blunt or fractures；The more bunchys of bast fiber, yellow green, fiber peripheral
Brilliant sheath fiber is formed containing calcium oxalate prismatic crystal in parenchyma cell, 16~26 μm of diameter；Amylum body is composite grain or simple grain, omphalion point
Shape, 3~8 μm of simple grain diameter；Conduit is bordered pit vessel, 31~52 μm of diameter；Cork cell's polygonal or similar round, it is pale brown
Color.
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