CN109765314A - A kind of method of quality control of butterflybush flower medicinal material - Google Patents
A kind of method of quality control of butterflybush flower medicinal material Download PDFInfo
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Abstract
The invention discloses a kind of method of quality control of butterflybush flower medicinal material, comprising the following steps: S1, measures the content of flavones ingredient and phenylethanoid glycoside in butterflybush flower medicinal material using HPLC-UV method；S2, with the total amount of flavones ingredient and phenylethanoid glycoside measured by flavones ingredient total amount measured by step (1) or phenylethanoid glycoside total amount or step (1), in conjunction with the peak area ratio of flavonoids representativeness ingredient and benzyl carbinol glycoside representativeness ingredient, as evaluation index, for evaluating the standard of butterflybush flower medical material quanlity and quality control, application of the above-mentioned method of quality control in the control of the quality of Flos Buddlejae extract and its preparation is additionally provided.Compared with prior art, the present invention reaches effective control to butterflybush flower medicinal material and its extract and the quality of the pharmaceutical preparations by controlling the content of two active components, the promotion to butterflybush flower series of products quality standard is realized, provides technical support to objectively evaluate butterflybush flower series of products quality.
Description
Technical field
The invention belongs to Analysis of Chinese Traditional Medicine fields, are related to a kind of method of quality control of Chinese medicine, and in particular to a kind of close illiteracy
The method of quality control of anther material.
Background technique
Butterflybush flower, alias cover flower, yellow meal flower, native brocade flower, sheep ear etc., are the dry of Loganiaceae Genus Buddleja L butterflybush flower
Dry bud and inflorescence.Butterflybush flower has wind-dispelling, and cool blood moistens liver, and improving eyesight and other effects can be used for treating red eye, swell pain, more tear photophobia,
The symptoms such as optic atrophy ocular.
The ingredients such as flavonoids, benzyl carbinol glycoside, terpene, volatile oil are mainly contained in butterflybush flower.Wherein flavonoids, benzyl carbinol
Glycoside is its main component, and flavones ingredient includes linarin, the new glycosides of butterflybush flower, apiolin, luteolin and its glycoside etc., benzene
Ethyl alcohol methods of glycosides includes verbascoside, Isoverbascoside, beta-hydroxy verbascoside, boschnaloside F, forsythiaside B, metal and stone silkworm
Glycosides etc..Modern research shows that the flavones ingredient in butterflybush flower has the effects that reducing blood lipid, liver protection, anti-inflammatory；Benzyl carbinol glycoside at
Dividing has the physiological activity such as antibacterial, anti-inflammatory, immunological regulation.Wherein, antibacterial, anti-inflammatory, quasi- hormone-like effect can be used for inhibiting inflammation
The factor, inhibition Apoptosis play quasi- hormone-like effect in conjunction with androgen receptor and come what the decline of therapeutic humoral level caused
Xerophthalmia；Aldose reductase inhibition activity can form cataract by preventing sorbierite from accumulating in texture；Liver protection simultaneously,
Hypoglycemic, immunoregulation effect can pass through maintenance blood glucose level, the development of enhancing immunity of organism delaying complications of diabetes；More than
Active constituent can significantly improve xerophthalmia and diabetic retinopathy symptom, move back screen effect with heat-clearing nourishing the liver, item and be consistent, can
It is considered as the material base for playing clinical efficacy.
With increasingly developed, the modern reason of the subjects such as pharmacy, biomedicine, chemistry, computer, mathematical statistics of science and technology
Tcm field constantly is penetrated by with science and technology, new scientific method and hand are provided for quality of medicinal material standard modern
Section establishes internationally recognized quality of medicinal material control and evaluation body with the raising year by year of the quality standard and supervision level of medicinal material
System, which has become, improves China's Chinese Medicine Industry competitiveness in the international market institute urgent problem to be solved.
Although pharmacopeia is described character, effect of butterflybush flower, compared with other conventional medicinal materials, it is more accurate to lack
Chemical qualitativity identify means and elementary item inspection, there is an urgent need to find that the basic chemical feature of medicinal material can be protruded more comprehensively
, can index ingredient associated with internal drug effect, and establish the method for quality control of system.
Chinese patent 20161025487.8 discloses a kind of method that ASE method extracts linarin in butterflybush flower, including with
Lower step: step 1: after butterflybush flower is crushed, sieving；Step 2: 0.5 parts by weight butterflybush flower powder is weighed, with 0.5 parts by weight diatom
Soil is uniformly mixed stand-by；Step 3: in the abstraction pool for putting filter membrane well in advance, suitable diatomite is added to reaching abstraction pool
Chi Kou；Cover the lid of abstraction pool；Step 4: ester is carried out to the mixture in abstraction pool；Step 5: right after step 4
Mixture in abstraction pool extracts；Extract liquor is obtained after extraction.
Chinese patent 201610254580.6 discloses a kind of measuring method of linarin in butterflybush flower, including following step
It is rapid: step 1: extract liquor being obtained by extraction using ASE extraction after butterflybush flower is crushed；Step 2: after extract liquor is centrifugated,
Obtain supernatant；Step 3: supernatant is analyzed using liquid chromatography.
Chinese patent 201410279787.X discloses a kind of application of butterflybush flower and extract in medicine preparation, should
Invention butterflybush flower is crushed after room temperature extract or be heated to reflux or supercritical extract in the extract that obtains, extraction made
Solvent is water and ethyl alcohol miscible liquid in any proportion；Either ether, petroleum ether, chloroform, ethyl acetate etc. have
Solvent miscible liquid in any proportion；Either liquid CO2。
Although coming real prior art discloses the method extracted the technique of linarin from butterflybush flower and measure Determination of Linarin
Now to the different sources even quality testing of the butterflybush flower medicinal material of different batches.But linarin is one kind in many medicinal materials
Common flavones ingredient is difficult to comprehensive, objective system evaluation butterflybush flower medicinal material only by the content of measurement linarin
And its quality of extract and preparation.It has not yet to see while using flavonoids and benzyl carbinol glycosides active component as quality control index
Multi objective measuring method is for effectively controlling the report of butterflybush flower quality of medicinal material comprehensively.
Summary of the invention
The purpose of the invention is to overcome the deficiencies in the prior art, are established using HPLC-UV method for measuring close illiteracy
Two kinds of linarin in anther material, two kinds of flavones ingredients of luteolin and verbascoside, Isoverbascoside benzyl carbinol glycoside chemistry
The method of quality control of component content, to being reached by the content for controlling two active components simultaneously to butterflybush flower medicinal material and its
Effective control of extract and the quality of the pharmaceutical preparations, it is close to objectively evaluate to realize the promotion to butterflybush flower series of products quality standard
It covers flower series of products quality and technical support is provided, to control butterflybush flower Related product quality and guarantee that curative effect is of great significance.
It explains:
1, there is not special instruction such as, " identical " being related in the present invention refers to the numerical value complete one with word index above-mentioned
It causes；" similar " or " close " that is related in the present invention refers to the number with the error of numerical value presence ± 1% of word index above-mentioned
Value.
2, there is not special instruction such as, water employed in the present invention is ultrapure water.
3, there is not special instruction such as, the % in the present invention is volumn concentration.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of method of quality control of butterflybush flower medicinal material, comprising the following steps:
S1, the content of flavones ingredient and phenylethanoid glycoside in butterflybush flower medicinal material is measured using HPLC-UV method；
S2, with Huang measured by flavones ingredient total amount measured by step (1) or phenylethanoid glycoside total amount or step (1)
The total amount of ketones component and phenylethanoid glycoside, in conjunction with the peak of flavonoids representativeness ingredient and benzyl carbinol glycoside representativeness ingredient
Area ratio, as evaluation index, for evaluating the standard of butterflybush flower medical material quanlity and quality control.
Preferably, flavones ingredient described in step S1 is linarin and luteolin.
Preferably, phenylethanoid glycoside described in step S2 is verbascoside and Isoverbascoside.
Preferably, flavonoids representative component described in step S2 is linarin.
Preferably, benzyl carbinol glycoside representativeness ingredient described in step S2 is verbascoside.
Preferably, flavones ingredient total amount described in step S2, phenylethanoid glycoside total amount, flavonoids and benzyl carbinol
Methods of glycosides total amount is arithmetic total amount or is the weight calculated after weighting.
Preferably, the step of HPLC-UV described in step (1) is measured are as follows:
(1) preparation of test solution；
Butterflybush flower medicinal material is weighed, addition volumetric concentration is 30%-100% methanol, it weighs again, after extracting 30-90min,
It is re-weighed, adding volumetric concentration is that 30%-100% methanol supplies reduced weight, it shakes up, through 0.45 μm of filtering with microporous membrane,
Taking subsequent filtrate is test solution；
(2) preparation of reference substance solution；
Linarin, luteolin, verbascoside and Isoverbascoside are weighed, mixing reference substance is obtained, into mixing reference substance
The methanol that volumetric concentration is 10%-100% is added, mixed reference substance solution is made；
(3) in sample flavones ingredient and phenylethanoid glycoside measurement；
The mixed reference substance solution that the test solution that takes step (1) to be prepared, step (2) are prepared is injected separately into
High performance liquid chromatograph is measured, and is obtained chromatogram, is calculated separately linarin, luteolin, feltwort by one point external standard method
The content of glycosides and Isoverbascoside.
It is further preferred that the condition that the high performance liquid chromatography measures are as follows:
Chromatographic column: reverse phase C18 chromatographic column；
Mobile phase: with acetonitrile for A phase, volumetric concentration is that 0.1% aqueous formic acid is B phase；
Gradient elution program are as follows: 0-100min, A phase: 98%-10%；B phase: 2%-90%；
Flow velocity: 1mL/min；
Detection wavelength: 330nm.
The present invention also provides above-mentioned method of quality control answering in the control of the quality of Flos Buddlejae extract and its preparation
With.
Preferably, the Flos Buddlejae extract is the water extract or ethanol extract of butterflybush flower medicinal material.
Compared with prior art, the invention has the benefit that
(1) traditional effect such as present invention selection and wind-dispelling, cool blood, profit liver, the improving eyesight of butterflybush flower is closely related, and content phase
To higher, representative linarin, luteolin, verbascoside and Isoverbascoside, totally 4 kinds of active constituents are used as measurement
The quality of butterflybush flower medicinal material can be effectively controlled in index.
(2) present invention for butterflybush flower medicinal material and its is mentioned by establishing flavonoids and benzyl carbinol glycoside chemical component index
Take object and preparation quality evaluation and quality control, more existing butterflybush flower quality of medicinal material standard only using a kind of ingredient of linarin as
Assay index can control the quality of butterflybush flower product more fully hereinafter.
(3) the HPLC-UV detection method that the present invention uses, quickly, easy, accuracy is good, can be objective, comprehensive, accurate
The quality of butterflybush flower medicinal material and its extract and preparation is evaluated on ground, to the quality of control butterflybush flower medicinal material and its extract and preparation
With guarantee that clinical efficacy is of great significance.
Specific embodiment
The present invention is furture elucidated combined with specific embodiments below, it should be understood that these embodiments be merely to illustrate the present invention and
It is not used in and limits the scope of the invention, after the present invention has been read, those skilled in the art are to various shapes of equal value of the invention
The modification of formula falls within the application range as defined in the appended claims.
A kind of method of quality control of butterflybush flower medicinal material, comprising the following steps:
S1, flavones ingredient linarin, luteolin and benzyl carbinol glycosides in butterflybush flower medicinal material are measured using HPLC-UV method
The content of constituents verbascoside and Isoverbascoside；
The step of HPLC-UV is measured are as follows:
(1) preparation of test solution；
Butterflybush flower medicinal material is weighed, addition volumetric concentration is 30%-100% methanol, it weighs again, after extracting 30-90min,
It is re-weighed, adding volumetric concentration is that 30%-100% methanol supplies reduced weight, it shakes up, through 0.45 μm of filtering with microporous membrane,
Taking subsequent filtrate is test solution；
(2) preparation of reference substance solution；
Linarin, luteolin, verbascoside and Isoverbascoside are weighed, mixing reference substance is obtained, into mixing reference substance
The methanol that volumetric concentration is 10%-100% is added, mixed reference substance solution is made；
(3) in sample flavones ingredient and phenylethanoid glycoside measurement；
The mixed reference substance solution that the test solution that takes step (1) to be prepared, step (2) are prepared is injected separately into
High performance liquid chromatograph is measured, and is obtained chromatogram, is calculated separately linarin, luteolin, feltwort by one point external standard method
The content of glycosides and Isoverbascoside.
The condition of the high performance liquid chromatography measurement are as follows:
Chromatographic column: reverse phase C18 chromatographic column；
Mobile phase: with acetonitrile for A phase, volumetric concentration is that 0.1% aqueous formic acid is B phase；
Gradient elution program are as follows: 0-100min, A phase: 98%-10%；B phase: 2%-90%；
Flow velocity: 1mL/min；
Detection wavelength: 330nm；
S2, with Huang measured by flavones ingredient total amount measured by step (1) or phenylethanoid glycoside total amount or step (1)
The total amount of ketones component and phenylethanoid glycoside, in conjunction with flavonoids representativeness ingredient linarin and benzyl carbinol glycoside representativeness at
The peak area ratio for dividing verbascoside, as evaluation index, for evaluating the standard of butterflybush flower medical material quanlity and quality control.
Preferably, flavones ingredient total amount described in step S2, phenylethanoid glycoside total amount, flavonoids and benzyl carbinol
Methods of glycosides total amount is arithmetic total amount or is the weight calculated after weighting.
The present invention also provides above-mentioned method of quality control answering in the control of the quality of Flos Buddlejae extract and its preparation
With.
Preferably, the Flos Buddlejae extract is the water extract or ethanol extract of butterflybush flower medicinal material.
Embodiment 1
A kind of method of quality control of butterflybush flower medicinal material, comprising the following steps:
S1, flavonoids and phenylethanoid glycoside measurement
(1) preparation of test solution
The butterflybush flower medicinal powder 0.5g for picking up from different sources, different batches is taken respectively, it is accurately weighed, it is respectively placed in
In 100mL stuffed conical flask, addition volumetric concentration be 80% methanol 50mL, close plug, accurately weighed weight, ultrasonic extraction 60min,
Accurately weighed weight again, adding volumetric concentration is that 80% methanol supplies reduced weight, is shaken up, through 0.45 μm of miillpore filter mistake
Filter, taking subsequent filtrate is test solution；
(2) preparation of reference substance solution
Linarin, luteolin, verbascoside and Isoverbascoside are taken, 80% methanol of volumetric concentration is added to be made containing linarin
The mixing of 50.25 μ g/mL, 50.08 μ g/mL of 50.19 μ g/mL of luteolin, 49.98 μ g/mL of verbascoside and Isoverbascoside
Contrast solution；
(3) in sample flavones ingredient and phenylethanoid glycoside measurement
The mixed reference substance solution that the test solution that takes step (1) to be prepared, step (2) are prepared is injected separately into
High performance liquid chromatograph is measured, and is obtained chromatogram, is calculated separately linarin, luteolin, feltwort by one point external standard method
The content of glycosides and Isoverbascoside.Measurement result is shown in Table 1.
The condition of above-described high performance liquid chromatography measurement are as follows:
Chromatographic column: Hypersil C18 chromatographic column (250mm × 4.6mm, 5 μm)
Mobile phase: with acetonitrile for A phase, volumetric concentration is that 0.1% aqueous formic acid is B phase；
Gradient elution program are as follows:
0-100min, A phase: 98%-10%；B phase: 2%-90%；
Flow velocity: 1mL/min
Detection wavelength: 330nm.
Flavonoids and benzyl carbinol glycoside primary efficacy chemical constituents determination result (%, n=3) in 1 butterflybush flower medicinal material of table
(4) butterflybush flower evaluation of medical materials' quality establishment of standard；
Respectively with the peak of flavonoids measured by step 1 and phenylethanoid glycoside total amount and linarin and Isoverbascoside
Area ratio is used to formulate the evaluation criterion of evaluation butterflybush flower medical material quanlity as evaluation index.
The present invention according to testing result, can provide reference standard are as follows: 6 batches of butterflybush flower medicine flavonoids that the present invention detects at
Dividing total amount average value is 1.12%, and phenylethanoid glycoside total amount average value is 1.30%, therefore, can be with flavones ingredient total amount
It is not less than 1.0% not less than 0.8%, phenylethanoid glycoside total amount, and linarin and verbascoside peak area ratio are in 0.5-3.0
Between assay limit standard as butterflybush flower medicinal material.
The present invention is used for butterflybush flower medicinal material and its extract by establishing flavonoids and benzyl carbinol glycoside chemical component index
It is controlled with the quality evaluation and quality of preparation, more existing butterflybush flower quality of medicinal material standard is only using a kind of ingredient of linarin as content
Testing index can control the quality of butterflybush flower product, while the HPLC-UV detection method that the present invention uses, fastly more fully hereinafter
Speed, easy, accuracy is good, can objective, comprehensive, accurately evaluate the quality of butterflybush flower medicinal material and its extract and preparation, right
It controls the quality of butterflybush flower medicinal material and its extract and preparation and guarantees that clinical efficacy is of great significance.
Claims (10)
1. a kind of method of quality control of butterflybush flower medicinal material, which comprises the following steps:
S1, the content of flavones ingredient and phenylethanoid glycoside in butterflybush flower medicinal material is measured using HPLC-UV method；
S2, with flavonoids measured by flavones ingredient total amount measured by step (1) or phenylethanoid glycoside total amount or step (1)
The total amount of ingredient and phenylethanoid glycoside, in conjunction with the peak area of flavonoids representativeness ingredient and benzyl carbinol glycoside representativeness ingredient
Ratio, as evaluation index, for evaluating the standard of butterflybush flower medical material quanlity and quality control.
2. method of quality control according to claim 1, which is characterized in that flavones ingredient described in step S1 is to cover
Flower glycosides and luteolin.
3. method of quality control according to claim 1, which is characterized in that phenylethanoid glycoside described in step S2
For verbascoside and Isoverbascoside.
4. method of quality control according to claim 1, which is characterized in that flavonoids representative component described in step S2
For linarin.
5. method of quality control according to claim 1, which is characterized in that benzyl carbinol glycoside described in step S2 represents
Property ingredient be verbascoside.
6. method of quality control according to claim 1, which is characterized in that flavones ingredient described in step S2 is total
Amount, phenylethanoid glycoside total amount, flavonoids and phenylethanoid glycoside total amount are arithmetic total amount or calculate after weighting
Weight.
7. method of quality control according to claim 1-6, which is characterized in that HPLC- described in step (1)
The step of UV is measured are as follows:
(1) preparation of test solution；
Butterflybush flower medicinal material is weighed, addition volumetric concentration is 30%-100% methanol, is weighed again, after extracting 30-90min, then is claimed
Weight, adding volumetric concentration is that 30%-100% methanol supplies reduced weight, shakes up, through 0.45 μm of filtering with microporous membrane, takes continuous
Filtrate is test solution；
(2) preparation of reference substance solution；
Linarin, luteolin, verbascoside and Isoverbascoside are weighed, mixing reference substance is obtained, is added into mixing reference substance
Volumetric concentration is the methanol of 10%-100%, and mixed reference substance solution is made；
(3) in sample flavones ingredient and phenylethanoid glycoside measurement；
The mixed reference substance solution that the test solution that takes step (1) to be prepared, step (2) are prepared is injected separately into efficiently
Liquid chromatograph is measured, obtain chromatogram, by one point external standard method calculate separately linarin, luteolin, verbascoside and
The content of Isoverbascoside.
8. method of quality control according to claim 7, which is characterized in that the condition of the high performance liquid chromatography measurement
Are as follows:
Chromatographic column: reverse phase C18 chromatographic column；
Mobile phase: with acetonitrile for A phase, volumetric concentration is that 0.1% aqueous formic acid is B phase；
Gradient elution program are as follows: 0-100min, A phase: 98%-10%；B phase: 2%-90%；
Flow velocity: 1mL/min；
Detection wavelength: 330nm.
9. method of quality control described in any one of claims 1-6 is in the control of the quality of Flos Buddlejae extract and its preparation
Using.
10. application according to claim 9, which is characterized in that the Flos Buddlejae extract is the water of butterflybush flower medicinal material
Extract or ethanol extract.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954380A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for linarin in Buddleja officinalis |
| CN108484695A (en) * | 2018-04-08 | 2018-09-04 | 湖南中医药大学 | A method of extracting benzyl carbinol glycosides and flavone compound simultaneously from butterflybush flower |
-
2019
- 2019-01-29 CN CN201910087776.4A patent/CN109765314A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954380A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for linarin in Buddleja officinalis |
| CN108484695A (en) * | 2018-04-08 | 2018-09-04 | 湖南中医药大学 | A method of extracting benzyl carbinol glycosides and flavone compound simultaneously from butterflybush flower |
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| 国家食品药品监督管理总局执业药师资格认证中心: "《中药学专业知识1》", 28 February 2015 * |
| 柴瑞平等: ""波长切换HPLC 同时测定车前草中5 个活性成分的含量", 《中国现代中药》 * |
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