CN110361346A - A kind of quality determining method of dendrobium candidum medicinal material - Google Patents
A kind of quality determining method of dendrobium candidum medicinal material Download PDFInfo
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- CN110361346A CN110361346A CN201910655781.0A CN201910655781A CN110361346A CN 110361346 A CN110361346 A CN 110361346A CN 201910655781 A CN201910655781 A CN 201910655781A CN 110361346 A CN110361346 A CN 110361346A
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- 150000002576 ketones Chemical class 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000000401 methanolic extract Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 244000138993 panchioli Species 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 206010036067 polydipsia Diseases 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- NLQLSVXGSXCXFE-UHFFFAOYSA-N sitosterol Natural products CC=C(/CCC(C)C1CC2C3=CCC4C(C)C(O)CCC4(C)C3CCC2(C)C1)C(C)C NLQLSVXGSXCXFE-UHFFFAOYSA-N 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
Abstract
The invention discloses a kind of quality determining methods of dendrobium candidum medicinal material, with the content of flavone c-glycoside in determined by ultraviolet spectrophotometry medicinal material, using flavone c-glycosides as reference substance, ultrasonic extraction, polar organic solvent and water-saturated n-butanol extraction in repeatedly using, total flavone c-glycosides are obtained, development process assay is then used.The method of the present invention is easy, easy, reproducible, it can definitely reflect the content of total flavone c-glycosides in dendrobium candidum medicinal material, the further perfect quality standard of dendrobium candidum medicinal material, it compensates in dendrobium candidum quality evaluation and lacks to using carbon glycosides flavones as the deficiency of the detection method of the flavonoids characteristic component of representative, keep the quality detection technology of dendrobium candidum medicinal material more scientific, reasonable.The quality of dendrobium candidum medicinal material can be effectively controlled using detection method of the present invention, so that it is guaranteed that the safety of its clinical application, stability and validity.
Description
Technical field
The invention belongs to pharmaceutical technology fields, are related to a kind of quality determining method of dendrobium candidum medicinal material.
Background technique
Dendrobium candidum is orchid family Dendrobium herbaceos perennial, and main medicinal part is fresh or dry stem, mainly
The ground such as Anhui, Zhejiang, Guangxi, Hunan, Yunnan, Guizhou are distributed in, are traditional rare traditional Chinese medicines.Dendrobium candidum has beneficial stomach raw
The effect of saliva, nourishing Yin and clearing heat, is used for impairment of yin body fluid deficiency, and dry polydipsia, deficiency of stomach-Yin, deficiency of food retch, abnormal heat is not moved back after being ill, deficiency of Yin fire
Prosperous, hectic fever due to yin labor heat, mesh is secretly unknown, the diseases such as muscles and bones impotence.Shennong's Herbal is classified as top grade, Taoism regimen classics " Taoist Scriptures "
It is described as first of " Chinese nine big mesonas ".
Pass through literature survey, the main pharmacological components and its feature of dendrobium candidum are as follows:
(1) polysaccharide (characteristic chemical constituent):
Polysaccharide is the main feature ingredient in dendrobium candidum, and relative molecular weight is in 10-70 ten thousand or so, predominantly D-
The heteroglycan that mannose and D-Glucose are polymerized.Various regions dendrobium candidum total starches content maintains 30% or so, and 2015 editions
States Pharmacopoeia specifications detection method and content requirement.
(2) volatile oil (characteristic chemical constituent):
Research about different sources volatile oil is few, and aliphatic accounts for relatively high, especially vapor steaming in volatile oil
When evaporating method, extract by solvents, aliphatic (such as oleic acid) accounts for 50% or more, content is higher have methyl linoleate (5.852%),
Pentacosane (10.132%), 22,23- dihydrostigmasterol (11.093%) and dioctyl adipate (21.115%) etc..Using
Solid-phase Microextraction, discovery main component are trans- 2- octenal (29.96%), alpha, beta-lonone (15.78%), linalool
(5.36%), aldehyde C-9 (4.39%), β-cyclocitral (3.40%) and n-capric aldehyde (3.14%) etc..
(3) stilbenes compound (Stilbenoids, characteristic chemical constituent, some of them are referred to as dendrobium nobile element), including a) simply connected
Benzyl class (also known as talan, Stilbene)；B) bibenzyl derivative species；C) luxuriant and rich with fragrance class (Phenanthrene).
Stilbenes compound is the characteristic chemical constituent in dendrobium candidum, but the research for carrying out assay to it is less.Chen Xian
The method (201410542575.6) for having invented bibenzyl assay such as good.Separately there is the careless dendrobium candidum scientific and technical innovation in Jiangxi nine to have
Limit company obtains preparation patent 1 (201610464044.9) of stilbenes compound active component.Agricultural University Of Anhui's application
A kind of method (201611261842.8) of dendrophnol in detection dendrobium candidum；Chongqing An Shang development in agricultural science and technology Co., Ltd
The method (201510660801.5) that erussian is extracted in dendrobium candidum is applied for.In three groups, ground according to Phytochemistry
Study carefully and HPLC detect multiple Bibenzyl compounds as a result, single bibenzyl content is high, bibenzyl derivative species content is taken second place, luxuriant and rich with fragrance class
Content is less.
(4) flavonoids, including flavanone (such as naringenin, non-characteristic chemical constituent), flavone c-glycoside (characteristic chemical constituent) etc..
Generally contain flavanone naringenin in dendrobium candidum, and naringenin is not the characteristic chemical constituent of dendrobium candidum,
It is largely present in orange peel, also by generally as plurality of Chinese and the quantitative ingredient of food, as Exocarpium Citri Grandis, Fructus Aurantii, dalbergia wood,
The dried immature fruit of citron orange, pine needle, shaddock, argy wormwood etc..
Flavone c-glycoside, be it is a kind of with carbon-carbon bond rather than the flavonoid glycoside compound of carbon-oxygen bond connection, structure has the characteristics that, is
The big polar characteristic chemical constituent of one kind present in dendrobium candidum.It has been found that having including schaftoside (schaftoside), different summer
About 10 kinds of flavone c-glycoside constituents of Buddhist support glycosides (isoschaftoside) etc., aglycon is apiolin.Zhejiang traditional Chinese medicine is big
It learns Lv Guiyuan etc. and is examined in the dendrobium candidum of Zhejiang including naringenin and the multiple compounds of flavone c-glycoside using finger-print
It surveys, the units such as Chinese department of traditional Chinese medicine institute, longevity celestial being paddy detect different sources flavone compound.The result shows that flavones
Class compound Regional differences, inter-species difference are more obvious.Zhejiang Dai Jun biological medicine Science and Technology Ltd. has applied for dendrobium candidum
The extracting method (201710249998.2) of middle chromocor compound, but non-flavone c-glycoside.Shanghai Univ. of Traditional Chinese Medicine obtains one kind
The thin-layer identification method patent of dendrobium candidum detects three kinds of flavone c-glycoside ingredients therein.(201410489539.8).
Not yet have been reported that the method for the total content of detection flavone c-glycoside constituents.For detection method, wherein HPLC,
HPLC-MS method detects the method for single or several flavone c-glycosides it has been reported that but relatively complicated.We have extensively studied with celery
Element is the property of the flavone c-glycoside of aglycon, establishes a kind of side based on ultraviolet, chemical reaction ultraviolet method measurement total flavone c-glycosides
Method, can dendrobium candidum carry out total flavone c-glycosides content detection, study the quality of dendrobium candidum.
(5) sesquiterpene alkaloids class (characteristic chemical constituent)
Though such components being characterized property ingredient, content is extremely low, and content is higher in other kind dendrobium nobiles.Agriculture of Anhui is big
Learn the detection method (201810469952.6) for having applied for a kind of dendrobium candidum total alkaloid content.
(6) lignans (glycosides) class (non-characteristic chemical constituent)
Lignans exist in various plants, and are not in groups in this kind, are non-characteristic chemical constituent.
(7) simple phenolic acid class (non-characteristic chemical constituent)
Including a variety of simple phenolic acid and its methods of glycosides, due to there are such components in various plants.
In conclusion the present invention is the flavone c-glycoside category feature ingredient contained in dendrobium candidum, carry out total flavone c-glycosides
Detection method of content research.
Flavone c-glycoside refer to sugar directly with flavones parent with the compound of C-C key joint, it is less in distributed in nature.Flavones
C-glycosides have been demonstrated with various actives (Wu Xinan, Zhao such as liver protection, anti-oxidant, antithyroid, desinsection, antiviral
The firm people, natural flavone carbon glycosides and its activity research progress, liberation army Acta Pharmaceutica Sinica, 2005,21,135-138), it is dendrobium candidum
One of effective component (Zhou Guifen, Lv Guiyuan and remove DPPH free radical energy at dendrobium candidum different parts flavone c-glycoside constituents
Power comparative studies, CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2012,37,1536-1540).The content of total flavone c-glycosides in dendrobium candidum is measured, it will
Help further to embody purposes of this kind of big polar character ingredient in terms of evaluation of medical materials' quality, it is scientific, comprehensively anti-to establish
The detection method for reflecting dendrobium candidum quality of medicinal material contributes.
Summary of the invention
The purpose of the present invention is to provide a kind of quality determining methods of dendrobium candidum medicinal material, relate generally to a kind of iron sheet stone
The detection method of content of total flavone c-glycosides in dry measure used in former times medicinal material, can be effectively controlled the quality of dendrobium candidum medicinal material, so that it is guaranteed that it is clinical
Safety, stability and the validity of application.
To achieve the above object, the present invention in dendrobium candidum by containing using apiolin as the flavone c-glycoside of aglycon
Series of studies, preferably extraction process, the hydrolysis process, the flavonoid glycoside coloration method that remove flavones oxygen glycosides etc., it is final provide it is as follows
Technical solution:
A kind of quality determining method of dendrobium candidum medicinal material, using total flavone c-glycosides in determined by ultraviolet spectrophotometry medicinal material
Content, using carbon glycosides flavone compound as reference substance, using high concentration alcohol water system ultrasonic extraction dendrobium candidum medicinal material, successively
It is extracted, n-butyl alcohol extract 1M methanol hydrochloride solution is hydrolyzed, then successively with middle polar organic solvent and water-saturated n-butanol
With middle polar organic solvent and water-saturated n-butanol extraction to obtain total flavone c-glycosides, then with triethylamine development process in 400nm
The assay of total carbon glycosides flavones is carried out with external standard method.
The quality determining method of the dendrobium candidum medicinal material, specific detecting step are as follows:
1) dendrobium candidum is crushed, crosses 80 meshes, it is 13- with weight/volume that precision, which measures 1g dendrobium candidum powder,
The high concentration alcohol water system ultrasonic extraction 10-60min of 100 times of amounts, filtration, residue are washed with solvent, and merging filtrate and washing lotion are set
In 100mL volumetric flask, constant volume.It shakes up, as extracting solution.
Precision measures 20mL extracting solution, is evaporated, and is redissolved with 10mL water, ultrasonic dissolution, transfer, then with 5mL water rinse, together
Transfer.It is extracted 3 times with polar organic solvent in 15mL, abandons organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase.
After being evaporated n-butanol phase, 20mL 1M methanol hydrochloride solution, the acidolysis 80min at 95 DEG C is added.It is evaporated acid solution, it is multiple with 10mL water
It is molten, ultrasonic dissolution, transfer, then use 5mL water rinse, shift together, using in 15mL polar organic solvent extract 3 times, abandoning it is organic
Phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase.
After being evaporated n-butanol phase, the dissolution of 60% EtOH Sonicate of 10mL is first added, adds 1% triethylamine solution of 10mL.
It is made into test liquid.
Said extracted with high concentration alcohol water system include but is not limited to concentration be 60%-95% methanol aqueous solution system,
Ethanol water system；Polar organic solvent includes but is not limited to chloroform, methylene chloride, ethyl acetate in above-mentioned extraction use
And their binary mixture.
2) preparation of reference substance solution: precision weighs the flavone c-glycosides standard control contained in dendrobium candidum
Product add the dissolution of 60% ethyl alcohol that solution is made；
Above-mentioned flavone c-glycosides reference substance, the including but not limited to dendrobium candidums such as Isoschaftoside, Schaftoside
In contain using apiolin as the flavone c-glycoside of aglycon.
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；Using ultraviolet spectrometry light
Degree method tests the absorbance at 400nm wavelength, and blank solution is noiseless；Content is calculated with calibration curve method.
As the further refinement scheme of the present invention: specific detecting step is as follows:
1) dendrobium candidum is crushed, crosses 80 meshes, precision measures 1g dendrobium candidum powder, is placed in conical flask, is added
90% methanol solution of 50mL, ultrasonic extraction 40min, filtration, residue are also washed with 90% methanol, and merging filtrate and washing lotion are placed in
100mL volumetric flask, constant volume.It shakes up, as extracting solution.
Precision measures 20mL extracting solution, is evaporated, and is redissolved with 10mL water, ultrasonic dissolution, transfer, then with 5mL water rinse flask,
It shifts together.It is extracted 3 times with 15mL chloroform, abandons organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase.It is evaporated just
After butanol phase, 20mL 1M methanol hydrochloride solution, the acidolysis 80min at 95 DEG C is added.It is evaporated acid solution, is redissolved with 10mL water, ultrasound
Dissolution, transfer, then 5mL water rinse flask is used, and it shifts, is extracted 3 times using 15mL chloroform together, abandoning organic phase, then with 15mL water
Saturation extracting n-butyl alcohol 3 times abandons water phase.
After being evaporated n-butanol phase, the dissolution of 60% EtOH Sonicate of 10mL is first added, adds 1% triethylamine solution of 10mL.
It is made into test liquid.
2) preparation of reference substance solution: precision weighs Isoschaftoside reference substance 4.7mg, is placed in 50mL volumetric flask, adds
The dissolution of 60% ethyl alcohol, constant volume, precision measure standard solution 0.5,1.0,1.5,2,3,4mL, and it is fixed to be respectively placed in 10mL volumetric flask
Hold to get reference substance solution；
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；According to ultraviolet spectrometry light
Degree method surveys absorbance at 400nm wavelength, and blank solution is noiseless；Content is calculated with calibration curve method, is vertical sit with absorbance
Y is marked, Isoschaftoside concentration is that abscissa X carries out linear regression, and acquiring regression equation is y=43.492x+0.0268, line
Property range be 0.00235mg/mL-0.0188mg/mL, coefficient R 2=0.996, linear relationship is good.
This detection method optimizes sample pre-treatments technique by single factor experiment, is recycled by precision, repeatability, sample-adding
The methods of learn verifying, it was demonstrated that be a kind of effective ways of total flavone c-glycosides in easy measurement dendrobium candidum.With prior art phase
Than, the beneficial effects of the present invention are: it is easy, easy, reproducible, it can definitely reflect dendrobium candidum quality of medicinal material, further
The perfect quality standard of dendrobium candidum medicinal material compensates in dendrobium candidum quality evaluation and lacks to using flavone c-glycoside as representative
The deficiency of the detection method of characteristic component keeps the quality detection technology of dendrobium candidum medicinal material more scientific, reasonable；Iron can be effectively controlled
The quality of skin dendrobium nobile medicinal material, so that it is guaranteed that the safety of its clinical application, stability and validity.
Detailed description of the invention
Fig. 1 is flavones oxygen glycosides (rutin) and flavone c-glycoside (Isoschaftoside) different condition sour water solution situation.
Fig. 2 is the relationship of carbon glycosides extracting flavonoids amount and extraction time.
Fig. 3 is carbon glycosides extracting flavonoids amount and the relationship for extracting solid-liquid ratio.
Fig. 4 is the relationship of carbon glycosides extracting flavonoids amount and extraction time.
Fig. 5 is Isoschaftoside canonical plotting.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1: Extraction solvent is investigated to be investigated with coloration method
The dendrobium candidum powder that 1g crosses 80 meshes is weighed, totally 5 parts, is denoted as A, B, C, D, E respectively；
A, 80% methanol ultrasonic extraction 40min of 20mL；B, 90% methanol ultrasonic extraction 40min of 20mL；C, 60% ethyl alcohol of 20mL
Ultrasonic extraction 40min；D, 80% EtOH Sonicate of 20mL extracts 40min；E, 95% EtOH Sonicate of 20mL extracts 40min, constant volume
To 25mL, extracting solution is obtained, 10mL test liquid is taken, is evaporated, is dissolved with 10mL water.Every time with 10mL water saturation ethyl acetate extraction three
It is secondary, abandon organic phase；Again three times with the extraction of 10mL water-saturated n-butanol, merge n-butanol phase, be evaporated, dissolved, obtained with 10mL methanol
Extract liquor.Extract liquor surveys absorbance value with following three kinds of methods.
NaNO2-Al(NO3)3- NaOH development process: 5mL prepare liquid is taken, 5%NaNO is added20.3mL places 5min after shaking,
Add 10%Al (NO3)30.3mL places 60min after shaking up, and adds 1.0mol/L NaOH 2mL, is settled to quarter with each corresponding solvent
Degree uses 1cm cuvette using zero pipe as blank after shaking up, absorbance is surveyed at 510nm.
The direct method of measurement: scanning measures under the absorbing wavelength after obtaining maximum absorption wavelength.
Triethylamine set process: taking reference substance solution 0.5mL, is placed in 5mL volumetric flask, adds Extraction solvent 2mL, with 1% triethylamine
Constant volume shakes up.Using reagent blank as reference, absorbance is measured in 400nm.
The results are shown in Table 1 for extraction:
The total carbon glycosides extracting flavonoids rate of 1 Different Extraction Method of table
90% methanol and 95% ethyl alcohol are owned by preferable effect of extracting as can be seen from the table, it is contemplated that compare ethyl alcohol, first
The polarity of alcohol is bigger, can preferably propose flavonoid glycoside.90% methanol of final choice is as Extraction solvent.
In measuring method, triethylamine set process needs to draw more reference substance solutions to increase absorbance value；Direct measuring method is every
It is secondary to scan maximum absorption wavelength, and in view of subsequent different batches dendrobium nobile sample may be in the content and type of flavone c-glycoside
On it is all variant, different batches maximum absorption wavelengths may be different, and it is shared more difficult to find out one, therefore does not use；NaNO2-Al
(NO3) 3-NaOH development process seems feasible, but finds that this method does not have the flavonoid glycoside purified after hydrolysis in subsequent experimental
Colour developing finds that this method colour developing principle is to two phenolic hydroxyl group of the neighbour colour developing in flavone aglycone, and dendrobium candidum by Literature Consult
In to be currently known contained carbon glycosides aglycon be apiolin, without adjacent two phenolic hydroxyl groups in apiolin, therefore do not use this method.Finally
Selection improves existing triethylamine chromogenic assay method.
Embodiment 2: the selection of wavelength is measured
By measurement reference substance and extract by triethylamine treated ultraviolet absorption maximum, as shown in table 2, determine
400nm is reasonable total carbon glycosides flavones determined by ultraviolet spectrophotometry wavelength.
The ultraviolet absorption maximum of 2 different material of table
| Reference substance/extract | Isoschaftoside | 90% methanol ultrasonic extraction processed material |
| Ultraviolet maximum absorption band/nm | 449,401,331 | 401,325,296.5 |
Embodiment 3: the selection of extractant
According to Literature Consult, discovery extracts flavones and water-saturated n-butanol is used to carry out depth extraction to flavones aqueous solution mostly
To obtain the higher flavones of purity.Removal oil-soluble impurities such as aglycon generally has ethyl acetate, chloroform, methylene chloride etc..I
When being tested using dendrobium candidum sample, TLC detection, discovery using ethyl acetate can be small by fraction polarity flavones
Glycosides is taken out of, and chloroform, methylene chloride are then not in such case, therefore the preferred chloroform of extractant or methylene chloride+water saturation
N-butanol.N-butanol extracting liquid carries out hydrochloric acid-magnesium powder reaction after being evaporated, be in aubergine, it was demonstrated that contain Huang in n-butanol extracting liquid
Ketone compounds.
Extraction times are equally probed into, and will be extracted obtained organic layer and directly be put on silica gel plate, are developed the color, observation
Whether contain Flavonoid substances, if so, then continuing to extract, determines that extraction times are 3 times.
Embodiment 4: the selection of Development of Thin-Layer Chromatography condition and acid hydrolysis conditions
4.1 Development of Thin-Layer Chromatography conditions
On polyamide film, use methanol: water: n-butanol=10:5:1 is as solvent, 1% aluminium chloride methanol reagent
For color developing agent.
4.2 hydrolysis temperature
300 μ g/mL rutin standard solution 5mL and 100 μ g/mL Isoschaftoside standard solution 1mL are measured, are added
20mL 1M methanol hydrochloride solution hydrolyzes 1h at 20,40,60,80,95 DEG C of different temperatures respectively, after being evaporated acid solution, 10mL first
Alcohol ultrasonic dissolution constant volume, Development of Thin-Layer Chromatography, observation hydrolysis situation.
4.3 concentration of hydrochloric acid
Measure 300 μ g/mL rutin standard solution 5mL and 100 μ g/mL Isoschaftoside standard solution 1mL, respectively plus
Entering 20mL methanol hydrochloride solution, concentration is respectively 0.2,0.4,0.6,0.8,1,1.2M, 1h is hydrolyzed at 95 DEG C, after being evaporated acid solution,
10mL methanol ultrasonic dissolution constant volume, Development of Thin-Layer Chromatography, observation hydrolysis situation.
4.4 hydrolysis time
Measure 300 μ g/mL rutin standard solution 5mL and 100 μ g/mL Isoschaftoside standard solution 1mL, respectively plus
Enter 20mL 1M methanol hydrochloride solution, hydrolyzes 20,40,60,80,100min at 95 DEG C, after being evaporated acid solution, 10mL methanol ultrasound is molten
Solve constant volume, Development of Thin-Layer Chromatography, observation hydrolysis situation.
By attached drawing 1 as it can be seen that number 1-5 is the thin-layer chromatography of sour water solution situation at 20,40,60,80,95 DEG C of different temperatures
Figure, it can be seen that rutin hydrolyzes completely substantially at 80 DEG C, to guarantee the hydrolysis of flavones oxygen glycosides completely, selects 95 DEG C of higher temperature；
Number 6-11 is the thin-layer chromatogram of sour water solution situation under different concentration of hydrochloric acid 0.2,0.4,0.6,0.8,1,1.2M, 0.8M hydrochloric acid
It can be seen that there are also minute quantities to remain under concentration, so selection 1M concentration of hydrochloric acid；Number 12-16 be different hydrolysis times 20,40,
60,80, under 100min sour water solution situation thin-layer chromatogram, it can be seen that there are also minute quantities to remain under 60min, base under 80min
This hydrolysis is complete, so selection hydrolysis time 80min.To sum up, acid hydrolysis conditions are that it is molten that 20mL1M hydrochloric acid methanol is added at 95 DEG C
Liquid hydrolyzes 80min.
Embodiment 5: experiment of single factor
5.1 extraction time
The dry stem powder of dendrobium candidum that 1g crosses 80 meshes is weighed, the methanol of 25mL90% is added, ultrasonic extraction is let cool,
Filtering, is settled to 100mL.Precision measures filtrate 20mL and measures A at 400nm, then read from regression equation after treatment
C out calculates to obtain carbon glycosides content, and obtained extraction time and the relationship of carbon glycosides extracting flavonoids rate are as shown in Fig. 2: 40-60min tri-
Person's extracted amount is very nearly the same, selects 40min, is 0.833mg/g.
5.2 liquid-to-solid ratio
The dry stem powder of dendrobium candidum that 1g crosses 80 meshes is weighed, the methanol of 13-100mL90%, ultrasonic extraction is added
40min is let cool, and filtering is settled to 100mL.Precision measures filtrate 20mL, after treatment, measures A at 400nm, then from returning
Return and read C on equation, calculates to obtain carbon glycosides extracting flavonoids rate, the relationship such as attached drawing 3 of obtained liquid-to-solid ratio and carbon glycosides extracting flavonoids rate
Shown: when liquid-to-solid ratio is 1:50, the recovery rate highest of carbon glycosides flavones is 0.894mg/g.
5.3 extraction time
The dry stem powder of dendrobium candidum that 1g crosses 80 meshes is weighed, the methanol of 50mL90% is added, ultrasonic extraction is multiple, puts
Cold, filtering, precision measures filtrate, is settled to 100mL, takes 20,100,100mL filtrates respectively, after treatment.?
A is measured at 400nm, then reads C from regression equation, calculates to obtain carbon glycosides extracting flavonoids rate, and obtained extraction time and carbon glycosides are yellow
The relationship of ketone recovery rate is as shown in Fig. 4: extracting 1 time can be presented above carbon glycosides flavones ingredient 90%.
Embodiment 6: methodological study
6.1 precision
The sample solution of same concentration, duplicate measurements A value 6 times calculate to obtain relative standard deviation as shown in table 3 at 400nm
=0.481%, show that instrument withinday precision is good.
The precision of 3 instrument of table
| Absorbance value | Flavones content (mg/g) | RSD |
| 0.330 | 0.7022 | |
| 0.333 | 0.7091 | |
| 0.334 | 0.7115 | 0.481% |
| 0.334 | 0.7115 | |
| 0.333 | 0.7091 | |
| 0.333 | 0.7091 |
6.2 repeated experiment
Weigh the dry stem powder of dendrobium candidum that 1g crosses 80 meshes, totally 6 parts.It is separately added into the methanol of 50mL90%, ultrasound
40min to be extracted, is let cool, filters, is settled to 100mL, precision measures filtrate 20mL, by processing, measure A at 400nm, then from
C is read on regression equation, calculates to obtain carbon glycosides flavones content, calculated result is as shown in table 4, calculates to obtain RSD=3.69%, shows the party
The repeatability of method is good.
4 repetitive test result of table
| Quality (g) | Absorbance value | Flavones content (mg/g) | RSD |
| 0.9969 | 0.370 | 0.7908 | |
| 1.0037 | 0.389 | 0.8297 | |
| 1.0051 | 0.404 | 0.8621 | 3.69% |
| 1.0034 | 0.379 | 0.8071 | |
| 1.0056 | 0.404 | 0.8625 | |
| 0.9984 | 0.399 | 0.8572 |
6.3 sample recovery rate
It is loaded recovery experiment
The dry stem powder of dendrobium candidum that 0.5g crosses 80 meshes is accurately weighed, totally 9 parts, is separately added into carbon glycosides flavonoid standards
In right amount, rate measurement is extracted by the preparation of above-mentioned test liquid and carbon glycosides flavones measuring method.As a result as shown in table 5 below.
Table 5 is loaded recovery test result
| Group | Quality (g) | Absorbance value | The rate of recovery | Average recovery rate | RSD |
| 0.4986 | 0.351 | 100.9% | |||
| Low (+3.2mL) | 0.5056 | 0.362 | 106.8% | 104.1% | 2.90% |
| 0.4974 | 0.356 | 104.7% | |||
| 0.5054 | 0.405 | 104.9% | |||
| In (+4mL) | 0.5066 | 0.382 | 96.3% | 99.2% | 4.98% |
| 0.5033 | 0.381 | 96.4% | |||
| 0.5065 | 0.425 | 100.8% | |||
| High (+4.8mL) | 0.5070 | 0.419 | 97.6% | 98.4% | 2.15% |
| 0.5014 | 0.415 | 96.8% |
6.4 stability experiment
Same test solution, dilution 50 times after, respectively 0,2h, 4h, 8h, for 24 hours with 48h measure A value, such as 11 institute of table
Show, gained relative standard deviation=4.40%, illustrates that test sample 48h internal stability is good.
Long-time stability sample is repeated experiment 2, is measured again after it is placed one month in refrigerator, absorbance
Value is 0.381.The RSD=1.47% compared with before, it was demonstrated that the sample placed one month in refrigerator is stable.
6 stability experiment result of table
| Time (h) | Absorbance value | Flavones content (mg/g) | RSD |
| 0 | 0.386 | 0.8869 | |
| 2 | 0.400 | 0.920 | |
| 4 | 0.386 | 0.8877 | 4.40% |
| 8 | 0.396 | 0.909 | |
| 24 | 0.417 | 0.958 | |
| 48 | 0.430 | 0.989 |
Embodiment 7: content assaying method
1) for sample liquid and preparation method thereof: dendrobium candidum is crushed, 80 meshes are crossed, precision measures 1g dendrobium candidum powder,
It is placed in conical flask, 90% methanol solution of 50mL is added, ultrasonic extraction 40min is filtered, and residue is also washed with 90% methanol, is closed
And filtrate and washing lotion, it is placed in 100mL volumetric flask, constant volume.It shakes up, as extracting solution.
Precision measures 20mL extracting solution, is evaporated, and is redissolved with 10mL water, ultrasonic dissolution, transfer, then with 5mL water rinse flask,
It shifts together.It is extracted 3 times with 15mL chloroform, abandons organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase.It is evaporated just
After butanol phase, 20mL 1M methanol hydrochloride solution, the acidolysis 80min at 95 DEG C is added.It is evaporated acid solution, is redissolved with 10mL water, ultrasound
Dissolution, transfer, then 5mL water rinse flask is used, and it shifts, is extracted 3 times using 15mL chloroform together, abandoning organic phase, then with 15mL water
Saturation extracting n-butyl alcohol 3 times abandons water phase.
After being evaporated n-butanol phase, the dissolution of 60% EtOH Sonicate of 10mL is first added, adds 1% triethylamine solution of 10mL.
It is made into test liquid
2) preparation of reference substance solution: precision weighs Isoschaftoside reference substance 4.7mg, is placed in 50mL volumetric flask, adds
The dissolution of 60% ethyl alcohol, constant volume, precision measure standard solution 0.5,1.0,1.5,2,3,4mL, and it is fixed to be respectively placed in 10mL volumetric flask
Hold to get reference substance solution；
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；According to ultraviolet spectrometry light
Degree method surveys absorbance at 400nm wavelength, and blank solution is noiseless；Content is calculated with calibration curve method, is vertical sit with absorbance
Y is marked, Isoschaftoside concentration is that abscissa X carries out linear regression, and acquiring regression equation is y=43.492x+0.0268, line
Property range be 0.00235mg/mL-0.0188mg/mL, coefficient R 2=0.996, linear relationship is good.Standard curve is shown in figure
5。
Embodiment 8: content assaying method
1) for sample liquid and preparation method thereof: dendrobium candidum is crushed, 80 meshes are crossed, precision measures 1g dendrobium candidum powder,
It is placed in conical flask, 80% ethanol solution of 50mL is added, ultrasonic extraction 50min is filtered, and residue also uses 80% ethanol washing, is closed
And filtrate and washing lotion, it is placed in 100mL volumetric flask, constant volume.It shakes up, as extracting solution.
Precision measures 20mL extracting solution, is evaporated, and is redissolved with 10mL water, ultrasonic dissolution, transfer, then with 5mL water rinse flask,
It shifts together.It is extracted 3 times with 15mL methylene chloride, abandons organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase.It steams
After dry n-butanol phase, 20mL 1M methanol hydrochloride solution, the acidolysis 80min at 95 DEG C is added.It is evaporated acid solution, is redissolved with 10mL water,
Ultrasonic dissolution, transfer, then use 5mL water rinse flask, shift together, using 15mL methylene chloride extract 3 times, abandoning organic phase, then
It is extracted 3 times with 15mL water-saturated n-butanol, abandons water phase.
After being evaporated n-butanol phase, the dissolution of 60% EtOH Sonicate of 10mL is first added, adds 1% triethylamine solution of 10mL.
It is made into test liquid
2) preparation of reference substance solution: precision weighs Schaftoside reference substance 5.0mg, is placed in 50mL volumetric flask, adds
The dissolution of 60% ethyl alcohol, constant volume, precision measure standard solution 0.5,1.0,1.5,2,3,4mL, and it is fixed to be respectively placed in 10mL volumetric flask
Hold to get reference substance solution；
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；According to ultraviolet spectrometry light
Degree method surveys absorbance at 400nm wavelength, and blank solution is noiseless；Content is calculated with calibration curve method, is vertical sit with absorbance
Y is marked, Schaftoside concentration is that abscissa X carries out linear regression, and acquiring regression equation is y=48.354x+0.0308, linearly
Range is 0.00250mg/mL-0.0200mg/mL, coefficient R 2=0.998, and linear relationship is good.
Embodiment 9: assay experiment
In method shown in embodiment 7, the total flavone c-glycosides content in a variety of dendrobium candidum samples is measured.
Weigh respectively 1g cross 80 meshes code name be SY-1, SY-2, GXD, GXL, GXS, KEB, XRC, WZTD, WZTY, WC,
The dry stem powder of the dendrobium candidum of LXX, HQ, NB, SXG, ZHH, TFTS, TFTH, TH, YLB, is added 90% methanol of 50mL,
1 40min of ultrasonic extraction, filtering, is settled to 100mL.Precision measures filtrate 20mL, after treatment.A is measured at 400nm,
Read C from the regression equation in embodiment 1 again, calculate recovery rate is as shown in table 12 below.
The area of the dendrobium candidum medicinal material of 7 different batches of table and planting type
The flavone c-glycoside content of the dendrobium candidum medicinal material of 8 different batches of table
By the above determination data it is found that content of the dendrobium candidum total flavone c-glycosides in various samples has notable difference, say
Bright this method can be used for distinguishing the quality of flavone c-glycoside in dendrobium candidum medicinal material.
The present invention is easy, easy, reproducible, can definitely reflect dendrobium candidum quality of medicinal material, further perfect iron
The quality standard of skin dendrobium nobile medicinal material compensates for the detection lacked in dendrobium candidum quality evaluation to the ingredient characterized by carbon glycosides flavones
The deficiency of method keeps the quality detection technology of dendrobium candidum medicinal material more scientific, reasonable；The matter of dendrobium candidum medicinal material can be effectively controlled
Amount, so that it is guaranteed that the safety of its clinical application, stability and validity.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (5)
1. a kind of quality determining method of dendrobium candidum medicinal material, which is characterized in that ultraviolet spectrophotometry is used, with dendrobium candidum
In the flavone c-glycosides that contain be reference substance, using high concentration alcohol water system ultrasonic extraction, successively use in polarity it is organic
Solvent and water-saturated n-butanol extraction, take n-butyl alcohol extract use again 1M methanol hydrochloride solution hydrolyze, then successively use in polarity have
Solvent and water-saturated n-butanol extraction are to obtain total flavone c-glycosides, finally with external standard method to the total flavone c-glycosides in dendrobium candidum
Carry out assay.
2. detection method according to claim 1, which is characterized in that specific detecting step is as follows:
1) dendrobium candidum is crushed, crosses 80 meshes, precision measures 1g dendrobium candidum powder, with weight/volume for 13-100 times
The high concentration alcohol water system ultrasonic extraction 10-60min of amount, filtration, residue are washed with solvent again, and merging filtrate and washing lotion are placed in
100mL volumetric flask, constant volume shake up, as extracting solution；
Take 20mL extracting solution, be evaporated, with 10mL water redissolve, ultrasonic dissolution, transfer, then use 5mL water rinse, shift together, use
Polar organic solvent extracts 3 times in 15mL, abandons organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandons water phase, be evaporated just
After butanol phase, 20mL1M methanol hydrochloride solution is added, acidolysis 80min, is evaporated acid solution at 95 DEG C, is redissolved with 10mL water, ultrasound
Dissolution, transfer, then 5mL water rinse is used, it shifts, is extracted 3 times using polar organic solvent in 15mL together, abandoning organic phase then is used
15mL water-saturated n-butanol extracts 3 times, abandons water phase；
After being evaporated n-butanol phase, the dissolution of 10mL60% EtOH Sonicate is first added, adds 10mL1% triethylamine solution, is made into confession
Test solution；
2) preparation of reference substance solution: taking flavone c-glycosides reference substance, adds the dissolution of 60% ethyl alcohol that solution is made；
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；Using uv-spectrophotometric
Method tests the absorbance at 400nm wavelength, and blank solution is noiseless；Content is calculated with calibration curve method.
3. detection method according to claim 2, which is characterized in that specifically detecting step is as follows:
1) dendrobium candidum is crushed, crosses 80 meshes, takes 1g dendrobium candidum powder, be placed in conical flask, 50mL90% methanol is added
Solution, ultrasonic extraction 40min, filtration, residue are also washed with 90% methanol solution, and merging filtrate and washing lotion are placed in 100mL capacity
Bottle, constant volume shakes up, as extracting solution；
Precision measures 20mL extracting solution, is evaporated, and is redissolved with 10mL water, ultrasonic dissolution, transfer, then with 5mL water rinse, turns together
It moves, is extracted 3 times with 15mL chloroform, abandon organic phase, then extracted 3 times with 15mL water-saturated n-butanol, abandon water phase, be evaporated n-butanol phase
Afterwards, 20mL1M methanol hydrochloride solution is added, acidolysis 80min, is evaporated acid solution at 95 DEG C, is redissolved with 10mL water, ultrasonic dissolution, turns
It moves, then uses 5mL water rinse flask, shift together, extracted 3 times using 15mL chloroform, abandoning organic phase, then with the positive fourth of 15mL water saturation
Alcohol extracts 3 times, abandons water phase,
After being evaporated n-butanol phase, the dissolution of 10mL60% EtOH Sonicate is first added, adds 10mL1% triethylamine solution, is made into confession
Test solution；
2) preparation of reference substance solution: precision weighs Isoschaftoside reference substance 4.7mg, is placed in 50mL volumetric flask, adds 60%
Ethyl alcohol dissolution, constant volume, precision measure standard solution 0.5,1.0,1.5,2,3,4mL, are respectively placed in constant volume in 10mL volumetric flask, i.e.,
Obtain reference substance solution；
3) measuring method: using 60% ethyl alcohol: 1% triethylamine=1:1 solution is blank reference solvent；According to ultraviolet spectrophotometry
Absorbance is surveyed at 400nm wavelength, blank solution is noiseless；Content is calculated with calibration curve method, using absorbance as ordinate Y,
Isoschaftoside concentration is that abscissa X carries out linear regression, and acquiring regression equation is y=43.492x+0.0268, linear model
It encloses for 0.00235mg/mL-0.0188mg/mL, coefficient R 2=0.996, linear relationship is good.
4. detection method according to claim 1 or 2, which is characterized in that the flavone c-glycoside contained in the dendrobium candidum
Class compound control product include but is not limited to Isoschaftoside, contain in Schaftoside dendrobium candidum using apiolin as aglycon
Flavone c-glycoside.
5. detection method according to claim 1 or 2, which is characterized in that the extraction high concentration alcohol water system includes
But it is not limited to the methanol aqueous solution system and ethanol water system system that concentration is 60%-95%；The middle polarity is organic molten
Agent includes but is not limited to chloroform, methylene chloride, ethyl acetate.
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