CN105136965B - The method of quality control of Fructus Corni and its extract with preparation and application - Google Patents
The method of quality control of Fructus Corni and its extract with preparation and application Download PDFInfo
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Abstract
The invention discloses a kind of Fructus Corni and its method for quality control of extract and preparation, the separate analytical technique that the present invention passes through high performance liquid chromatography, 3 iridoid glycosideses and 2 methods of triterpene acids chemical composition are determined by setting up, the quality control to Fructus Corni and its extract and preparation is realized.The method with two active components in extract to Fructus Corni and its preparation by being analyzed simultaneously, compare with single analysis some or a certain class chemical composition, can comprehensive, objective, effective evaluation Fructus Corni and its extract and preparation quality, and for its quality control, and the method is easy to operate, good stability, it is easy to promote.
Description
Technical field
The present invention relates to a kind of Chinese medicine and its method for quality control of preparation, and in particular to Fructus Corni and its extraction
The method of quality control of thing and preparation.
Background technology
Fructus Corni is the drying and ripening of Cornaceae plant Fructus Corni Cornus officinalis Sieb.et Zucc.
Pulp, is widely used in tcm clinical practice, and with tonifying the liver and kidney, the work(of arresting collape syndrome by astringents is usually used in dizziness and tinnitus, soreness of waist and knee joint, sun
The diseases such as impotence seminal emission, enuresis frequent micturition, uterine bleeding under band, profuse sweating collapse, Heat Diabetes.Modern study shows, chemistry contained by Fructus Corni into
It is point complex, mainly contain iridoid glycosides, triterpene acids, flavonoids, organic acid and its esters, polysaccharide etc..Wherein,
Iridoid glycosides chemical composition has reduces the bioactivity such as blood sugar, immune enhancing, diuresis, step-down, anti-inflammatory, neuroprotection,
Triterpene acids chemical composition has the bioactivity such as immune enhancing, liver protection, hypoglycemic, antitumor, both at Fructus Corni
Play the main matter basis of traditional effect.Current document report is more with cyclenes ether about the method for quality control of Fructus Corni
Terpene glycoside or organic acid chemical composition as primary evaluation index, and《Chinese Pharmacopoeia》Version is only recorded with loganin list within 2010
One composition as Fructus Corni assay index, it is difficult to comprehensively, objectively be used for evaluate Fructus Corni and its extraction
The quality of thing and preparation.Have not yet to see many fingers simultaneously with iridoid glycosides and triterpenic acid active component as quality control index
Mark assay method is used for comprehensively the effectively report of control Fructus Corni quality.
The content of the invention
Goal of the invention：The invention aims to overcome the deficiencies in the prior art, HPLC-UV, HPLC- is respectively adopted
ELSD methods are set up for determining morroniside, loganin, three kinds of iridoid glycosideses of chiratin and olive in Fructus Corni
Acid, two kinds of method of quality control of triterpene acids chemical composition content of ursolic acid, to pass through to control two active components simultaneously
Content reach effective control to Fructus Corni and its extract and the quality of the pharmaceutical preparations, to realize Fructus Corni series of products quality
The lifting of standard, for objective evaluation Fructus Corni series of products quality provides technical support, to control Fructus Corni Related product quality
It is significant with guarantee curative effect.
Technical scheme：In order to realize the above object the technical scheme that the present invention takes is：
A kind of Fructus Corni and its extract and the method for quality control of preparation, comprise the following steps：
(1) Fructus Corni and its extract are determined with morroniside, loganin, chiratin 3 in preparation using HPLC-UV methods
Plant the content of iridoid glycosides chemical composition；
(2) Fructus Corni and its extract are determined with ursolic acid, 2 kinds of oleanolic acid in preparation using HPLC-ELSD methods
The content of triterpene acids chemical composition；
(3) it is total with iridoid constituents total amount, Triterpene acids measured by step (2) measured by step (1) respectively
Amount, or step (1) and step (2) determine iridoids and Triterpene acids total amount as evaluation index for making
Accepted opinion valency Fructus Corni and its extract are with preparation quality and carry out the standard of quality control.
Preferably, the method for quality control of above-described Fructus Corni and its extract and preparation, step
(1) the step of HPLC-UV described in is determined be：
(1) preparation of need testing solution
Fructus Corni or its extract or appropriate preparation are taken, it is accurately weighed, it is placed in conical flask with cover, precision adds body
Product concentration is 40%~80% methyl alcohol, and close plug, weighed weight extracts 60~120min, then weighed weight, plus volumetric concentration 40%
~80% methyl alcohol supplies the weight of less loss, shakes up, and after being filtered through 0.45 μm of miillpore filter, takes subsequent filtrate, obtains final product test sample molten
Liquid；
(2) preparation of reference substance solution
Take morroniside, loganin, chiratin reference substance each appropriate, plus the methyl alcohol of volumetric concentration 40%~80% is made and contains respectively
The μ gmL of morroniside 50-1, the μ gmL of loganin 50-1, the μ gmL of chiratin 20-1Mixed reference substance solution；
(3) in sample iridoid glycosides active component measure
The mixed reference substance solution that the need testing solution, step (2) that step (1) prepares prepare is taken to be injected separately into
High performance liquid chromatograph is measured, and obtains chromatogram, and morroniside, loganin, chiratin are calculated by one point external standard method respectively
Mass concentration；
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Anti-phase C18 chromatographic columns；
Mobile phase：It is A phases with acetonitrile, the aqueous formic acid of volumetric concentration 0.1% is B phases, gradient elution；
Flow velocity：0.8mL/min~1mL/min；
Detection wavelength：235~245nm.
Preferably, the method for quality control of above-described Fructus Corni and its extract and preparation, step
(2) the step of HPLC-ELSD described in is determined be：
(1) preparation of need testing solution
Fructus Corni or its extract or appropriate preparation are taken, it is accurately weighed, it is placed in conical flask with cover, precision adds body
Product concentration is 60%~100% methyl alcohol or ethanol, and close plug, weighed weight extracts 60~120min, then weighed weight, plus volume
Concentration is the weight that 60%~100% methyl alcohol or ethanol supply less loss, is shaken up, and after being filtered through 0.45 μm of miillpore filter, is taken continuous
Filtrate, obtains final product.
(2) preparation of reference substance solution
Take oleanolic acid, ursolic acid reference substance appropriate, plus methyl alcohol is made the μ gmL containing oleanolic acid 100 respectively-1, ursolic acid
200μg·mL-1Mixed reference substance solution, obtain final product；
(3) in sample triterpene acids active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into height
Effect liquid phase chromatogram instrument is measured, and obtains chromatogram, and oleanolic acid, ursolic acid are calculated respectively by external standard logarithmic equation two-point method
Mass concentration；
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Anti-phase C18 chromatographic columns；
Mobile phase：Volume ratio is 17：83 0.5% acetic acid amine aqueous solution and methyl alcohol；
Flow velocity：0.6~0.8mL/min；
ELSD detects atomizer temperature：80~100 DEG C, carrier gas flux：2.7~3.0L/min.
Preferably, the method for quality control of above-described Fructus Corni and its extract and preparation, step
(3) iridoid constituents total amount, Triterpene acids total amount, iridoids and Triterpene acids total amount described in can be
The total amount calculated after arithmetic total amount, or weighting.
Preferably, the method for quality control of above-described Fructus Corni and its extract and preparation, step
(3) described in can be 5 compositions (3 iridoidses and 2 for formulating evaluation sample quality and carrying out the standard of quality control
Triterpene acids) total amount, or 3 iridoid constituents total amounts or 2 Triterpene acids total amounts totally three fingers
Mark is collectively as evaluation index.
As more preferably scheme, the method for quality control of above-described Fructus Corni and its extract and preparation, its
It is characterised by, described iridoid glycosides active component determines eluent gradient elution program and is：0~20min, 10%-
17% acetonitrile, 0.1% aqueous formic acid 90%-83%.
Preferably, the method for quality control of above-described Fructus Corni and its extract and preparation, step
(1), the cornel extractive described in step (2) is the water extract or ethanol extract of Fructus Corni.
The present invention choose with Fructus Corni have tonify the liver and kidney, the tradition effect such as arresting collape syndrome by astringents it is closely related, and content phase
To higher, representative morroniside, loganin, chiratin and oleanolic acid, ursolic acid totally 5 kinds of active components as measure
Index, can effectively control the quality of Fructus Corni.
Morroniside, loganin, 3 kinds of iridoids chemical compositions of chiratin, its λ that the present invention is determinedmaxRespectively
240th, 238,246nm, for ease of analysis and the popularization of method, therefore using 235~245nm as determining wavelength, and preferably 240nm makees
To determine wavelength.Screening by being unable to flow velocity of the invention, it is determined that optimal flow velocity is 1mL/min.
2 kinds of triterpenic acid active components of oleanolic acid and ursolic acid that the present invention is determined are because of its UV absorption for end is inhaled
Receive, during using UV detectors, baseline interference is larger, therefore selects EISD, to reduce interference.Additionally, olive
Acid is isomer with ursolic acid, and its physico-chemical property is more similar, there is certain difficulty in chromatographic separation process.This hair
It is bright to have screened the influence of different flow phase systems and chromatographic column to its separating effect by many experiments.It is final preferably with methyl alcohol-
0.5% ammonium acetate solution has good separating effect as flow phase system, and low flow velocity, low column temperature are conducive to targeted
Compound is efficiently separated.The present invention screens different chromatographic columns, screening test result table further through many experiments under this systems
It is bright, with Hypersil C18Chromatographic column has optimal separating effect.
Beneficial effect：Fructus Corni and its method for quality control and existing skill of extract and preparation that the present invention is provided
Art is compared to advantages below：
The present invention is sieved according to active component in Fructus Corni and the structural property feature of impurity component by many experiments
Choosing, with iridoid glycosides and triterpene acids chemical composition as index while foundation, for Fructus Corni and its extract
Quality evaluation and quality control with preparation, more existing Fructus Corni quality standard is only using a kind of composition of loganin as content
Testing index, can more fully hereinafter control the quality of Fructus Corni product.
The present invention is screened by many experiments and obtains optimal mobility composition, elution program, chromatographic column, flow velocity, detection
The chromatographic conditions such as device, method that the present invention sets up is quick, the easy, degree of accuracy is good, can with it is objective, comprehensive, evaluate mountain exactly
Fruit of medicinal cornel medicinal material and its extract and the quality of preparation, face control Fructus Corni and its extract with the quality of preparation and guarantee
Bed curative effect is significant.
Brief description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram that iridoid glycosides active component mixes reference substance (A) and sample (B).
Fig. 2 is the high-efficient liquid phase chromatogram that triterpene acids active component mixes reference substance (A) and sample (B).
Specific embodiment
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments be merely to illustrate the present invention and
Limitation the scope of the present invention is not used in, 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 appended claims limited range.
Embodiment 1
1. the measure of iridoid glycoside constituents
(1) preparation of need testing solution
Fructus Corni (being shown in Table 1) powder (40 mesh) the about 0.4g for picking up from different sources, different batches is taken respectively, and precision claims
It is fixed, it is respectively placed in 100mL conical flask with cover, precision adds 60% methyl alcohol 50mL, close plug, weighed weight, room temperature ultrasound
(40kHz) extracts 60min, then weighed weight, plus 60% methyl alcohol supplies the weight of less loss, shakes up, through 0.45 μm of miillpore filter
After filtration, subsequent filtrate is taken, obtain final product the Fructus Corni need testing solution of 13 different sources and batch.
(2) preparation of reference substance solution
Take morroniside, loganin, chiratin reference substance each appropriate, plus 60% methyl alcohol is made the μ containing morroniside 53.35 respectively
g·mL-1The μ gmL of loganin 55.15-1, the μ gmL of chiratin 19.92-1Mixed reference substance solution, obtain final product.
(3) in sample iridoid glycosides active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into height
Effect liquid phase chromatogram instrument is measured, and obtains chromatogram, calculates the matter of morroniside, loganin, chiratin respectively by one point external standard method
Amount concentration, measurement result is shown in Table 1.
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Alltima C18Chromatographic column (250mm × 4.6mm, 5 μm)；
Mobile phase：The aqueous formic acid (B) of acetonitrile (A) -0.1% is eluted for eluent gradient：0~20min, 10%-17%
Acetonitrile (A), 90~83% 0.1% aqueous formic acid (B)；
Flow velocity：1mL/min；
Detection wavelength：240nm
2. the measure of Triterpene acids
(1) preparation of need testing solution
Fructus Corni (being shown in Table 1) powder (40 mesh) the about 1g for picking up from different sources, different batches is taken respectively, it is accurate respectively
It is weighed, it is placed in 50mL conical flask with cover, precision adds methyl alcohol 20mL, and close plug, weighed weight, room temperature ultrasound (40kHz) is extracted
60min, then weighed weight, plus methyl alcohol supply the weight of less loss, shake up, and after being filtered through 0.45 μm of miillpore filter, take subsequent filtrate,
Obtain final product the Fructus Corni need testing solution of 13 different sources and batch.
(2) preparation of reference substance solution
Take oleanolic acid, ursolic acid reference substance appropriate, plus methyl alcohol is made the μ gmL containing oleanolic acid 154.8 respectively-1, black bearberry
216.4 μ gmL of acid-1Mixed reference substance solution, obtain final product.
(3) in sample triterpene acids active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into height
Effect liquid phase chromatogram instrument is measured, and obtains chromatogram, and oleanolic acid, ursolic acid are calculated respectively by external standard logarithmic equation two-point method
Mass concentration, measurement result is shown in Table 1.
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Hypersil C18Chromatographic column (250mm × 4.6mm, 5 μm)；
Mobile phase：The ammonium acetate of methyl alcohol -0.5% (83:17)；
Flow velocity：0.6mL/min；
ELSD detects atomizer temperature：80 DEG C, carrier gas flux：2.7L/min.
Iridoid glycosides and triterpene acids primary efficacy chemical constituents determination result (%, n=in the Fructus Corni of table 1
3)
3. the foundation of Fructus Corni criteria of quality evaluation
Respectively with iridoid constituents total amount, Triterpene acids total amount measured by step 2 measured by step 1, as
Evaluation index is used to formulate the evaluation criterion for evaluating Fructus Corni quality.
According to testing result, can provide reference standard is the present invention：13 batches of Fructus Corni cyclenes of present invention detection
Ether terpene glycosides total amount average value is 2.15%, and triterpenic acid total amount average value is 0.33%, therefore can be not low with iridoid glycoside total amount
0.25% is not less than as the assay limit standard for Fructus Corni in 1.7%, triterpenic acid total amount.
Embodiment 2
1. the preparation of cornel extractive
(1) preparation of Fructus Corni water extract
The Fructus Corni 2kg for picking up from Henan Xixia Mine is taken, the 20L refluxing extractions that add water respectively 2 times, each 2h, filtering, filtrate
It is recovered under reduced pressure to 5L, plus ethanol is staticly settled to alcohol content up to 80%, supernatant reclaims ethanol, and evaporated under reduced pressure obtains Fructus Corni water
Extract A 0.45kg.
The Fructus Corni 1kg for picking up from Zhejiang Chunan separately is taken, the 10L refluxing extractions that add water respectively 2 times, each 2h, filtering, filter
Liquid is recovered under reduced pressure to 2L, plus ethanol is staticly settled to alcohol content up to 80%, and supernatant reclaims ethanol, and evaporated under reduced pressure obtains Fructus Corni
Water extract B 0.21kg.
(2) preparation of Fructus Corni ethanol extract
The Fructus Corni 2kg for picking up from Henan Xixia Mine is taken, adds ethanol 20L refluxing extractions 2 times respectively, each 2h, filtering, filter
Liquid reclaims ethanol, and evaporated under reduced pressure obtains Fructus Corni ethanol extract A 0.32kg.
The Fructus Corni 1kg for picking up from Zhejiang Chunan separately is taken, adds ethanol 10L refluxing extractions 2 times respectively, each 2h, filtering,
Filtrate recycling ethanol, evaporated under reduced pressure obtains Fructus Corni ethanol extract B 0.15kg.
2.2. the measure of iridoid glycoside constituents
(1) preparation of need testing solution
The poly- 1 gained Fructus Corni water extract of step and ethanol extract (0.1g) are taken respectively, it is accurately weighed, it is placed in 100mL tools
In plug conical flask, precision adds 50% methyl alcohol 50mL, and close plug, weighed weight, room temperature ultrasound (40kHz) extracts 60min, then weighed
Weight, plus 50% methyl alcohol supplies the weight of less loss, shakes up, and after being filtered through 0.45 μm of miillpore filter, takes subsequent filtrate, obtains final product.
(2) preparation of reference substance solution
Take morroniside, loganin, chiratin reference substance each appropriate, plus 50% methyl alcohol is made the μ containing morroniside 50.10 respectively
g·mL-1The μ gmL of loganin 50.05-1, the μ gmL of chiratin 19.95-1Mixed reference substance solution, obtain final product.
(3) in sample iridoid glycosides active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into height
Effect liquid phase chromatogram instrument is measured, and obtains chromatogram, calculates the matter of morroniside, loganin, chiratin respectively by one point external standard method
Amount concentration, measurement result is shown in Table 2.
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Alltima C18Chromatographic column (250mm × 4.6mm, 5 μm)；
Mobile phase：The aqueous formic acid (B) of acetonitrile (A) -0.1% is eluted for eluent gradient：0~20min, 12%-17%
A；
Flow velocity：1mL/min；
Detection wavelength：238nm.
2. the measure of Triterpene acids
(1) preparation of need testing solution
The poly- 1 gained Fructus Corni water extract of step, ethanol extract each 0.25g are taken respectively, it is accurately weighed, it is placed in 50mL tool plugs
In conical flask, precision adds methyl alcohol 20mL, and close plug, weighed weight, room temperature ultrasound (40kHz) extracts 60min, then weighed weight,
Plus methyl alcohol supplies the weight of less loss, shakes up, after being filtered through 0.45 μm of miillpore filter, subsequent filtrate is taken, obtained final product.
(2) preparation of reference substance solution
Take oleanolic acid, ursolic acid reference substance appropriate, plus methyl alcohol is made the μ gmL containing oleanolic acid 100.2 respectively-1, black bearberry
205.2 μ gmL of acid-1Mixed reference substance solution, obtain final product.
(3) in sample triterpene acids active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into height
Effect liquid phase chromatogram instrument is measured, and obtains chromatogram, and oleanolic acid, ursolic acid are calculated respectively by external standard logarithmic equation two-point method
Mass concentration, measurement result is shown in Table 2.
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Hypersil C18Chromatographic column (250mm × 4.6mm, 5 μm)；
Mobile phase：The ammonium acetate of methyl alcohol -0.5% (83:17)；
Flow velocity：0.6mL/min；
ELSD detects atomizer temperature：80 DEG C, carrier gas flux：2.7L/min.
Iridoid glycosides and triterpene acids primary efficacy chemical constituents determination result (%, n in the cornel extractive of table 1
=3)
3. the foundation of cornel extractive criteria of quality evaluation
Respectively with iridoid constituents total amount, Triterpene acids total amount measured by step 2 measured by step 1, and
Iridoid glycoside is used to formulate the evaluation criterion for evaluating Fructus Corni quality with triterpenic acid total amount as evaluation index.
Accordingly, according to testing result, can provide reference standard is the present invention：Fructus Corni water extract iridoid glycoside is total
Must not measure less than 7.45%, triterpenic acid total amount must not be less than 1.15%, and the two total amount must not be less than 8.60%；Regulation cornusol
Extract iridoid glycoside total amount must not be less than 7.28%, and triterpenic acid total amount must not be less than 1.88%, and the two total amount must not be less than
9.21%.
Above test result indicate that, Fructus Corni and its method for quality control of extract and preparation that the present invention is provided
It is used for the product of Fructus Corni and its extract and preparation as index with iridoid glycosides and triterpene acids chemical composition simultaneously
Matter evaluate and quality control, more existing Fructus Corni quality standard only using a kind of composition of loganin as assay index,
More can comprehensively control the quality of Fructus Corni product.And the method set up is quick, the easy, degree of accuracy is good, can be with objective, complete
Face, the quality for evaluating Fructus Corni and its extract and preparation exactly, to control Fructus Corni and its extract and system
The quality and guarantee clinical efficacy of agent are significant.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (4)
1. the method for quality control of a kind of Fructus Corni and its extract and preparation, it is characterised in that comprise the following steps：
(1) Fructus Corni and its extract are determined with morroniside, loganin, 3 kinds of rings of chiratin in preparation using HPLC-UV methods
The content of alkene ether terpene glycoside chemical components；
(2) Fructus Corni and its extract are determined with ursolic acid, 2 kinds of triterpenes of oleanolic acid in preparation using HPLC-ELSD methods
The content of acids chemical composition；
(3) respectively with iridoid constituents total amount, Triterpene acids total amount measured by step (2) measured by step (1), or
Person's step (1) and step (2) determine the iridoids and Triterpene acids total amount for obtaining, and are used to make as evaluation index
Accepted opinion valency Fructus Corni and its extract are with preparation quality and carry out the standard of quality control；
The step of HPLC-UV described in step (1) is determined be：
(1) preparation of need testing solution
Fructus Corni or its extract or appropriate preparation are taken, it is accurately weighed, it is placed in conical flask with cover, precision adds volume dense
It is 40%~80% methyl alcohol to spend, close plug, weighed weight, 60~120min of extraction, then weighed weight, plus volumetric concentration 40%~
80% methyl alcohol supplies the weight of less loss, shakes up, and after being filtered through 0.45 μm of miillpore filter, takes subsequent filtrate, obtains final product need testing solution；
(2) preparation of reference substance solution
Take morroniside, loganin, chiratin reference substance each appropriate, plus the methyl alcohol of volumetric concentration 40%~80% is made and contains Monot respectively
The μ gmL of glycosides 50-1, the μ gmL of loganin 50-1, the μ gmL of chiratin 20-1Mixed reference substance solution；
(3) in sample iridoid glycosides active component measure
The mixed reference substance solution that the need testing solution, step (2) that step (1) prepares prepare is taken to be injected separately into efficiently
Liquid chromatograph is measured, and obtains chromatogram, calculates the quality of morroniside, loganin, chiratin respectively by one point external standard method
Concentration；
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Anti-phase C18 chromatographic columns；
Mobile phase：It is A phases with acetonitrile, the aqueous formic acid of volumetric concentration 0.1% is B phases, gradient elution；Gradient elution program is：0
~20min, 10%-17% acetonitrile, 0.1% aqueous formic acid 90%-83%；
Flow velocity：1mL/min；
Detection wavelength：240nm；
The step of HPLC-ELSD described in step (2) is determined be：
(1) preparation of need testing solution
Fructus Corni or its extract or appropriate preparation are taken, it is accurately weighed, it is placed in conical flask with cover, precision adds volume dense
It is 60%~100% methyl alcohol or ethanol to spend, and close plug, weighed weight extracts 60~120min, then weighed weight, plus volumetric concentration
The weight of less loss is supplied for 60%~100% methyl alcohol or ethanol, is shaken up, after being filtered through 0.45 μm of miillpore filter, take subsequent filtrate,
Obtain final product；
(2) preparation of reference substance solution
Take oleanolic acid, ursolic acid reference substance appropriate, plus methyl alcohol is made the μ gmL containing oleanolic acid 100 respectively-1, the μ of ursolic acid 200
g·mL-1Mixed reference substance solution, obtain final product；
(3) in sample triterpene acids active component measure
Take the mixed reference substance solution that the sample solution, step (2) that step (1) prepares prepare and be injected separately into efficient liquid
Chromatography is measured, and obtains chromatogram, calculates the quality of oleanolic acid, ursolic acid respectively by external standard logarithmic equation two-point method
Concentration；
The condition that above-described high performance liquid chromatography is determined is：
Chromatographic column：Anti-phase C18 chromatographic columns, chromatographic column filler model Hypersil C18；
Mobile phase：Volume ratio is 17：83 0.5% acetic acid amine aqueous solution and methyl alcohol；
Flow velocity：0.6mL/min；
ELSD detects atomizer temperature：80 DEG C, carrier gas flux：2.7L/min.
2. the method for quality control of Fructus Corni according to claim 1 and its extract and preparation, it is characterised in that
Iridoid constituents total amount, Triterpene acids total amount, iridoids and Triterpene acids total amount described in step (3)
For arithmetic total amount or be after weighting calculate total amount.
3. the method for quality control of Fructus Corni according to claim 1 and its extract and preparation, it is characterised in that
Described in step (3) for formulate evaluate sample quality and carry out quality control standard be 3 iridoidses and 2 triterpenic acids
Constituents totally 5 compositions, or be 3 iridoid constituents total amounts or 2 Triterpene acids total amounts.
4. the method for quality control of Fructus Corni according to claim 1 and its extract and preparation, it is characterised in that
Cornel extractive described in step (1), step (2) is the water extract or ethanol extract of Fructus Corni.
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| CN105974029B (en) * | 2016-07-11 | 2018-02-27 | 山东省分析测试中心 | Method that is a kind of while determining six kinds of iridoid glycoside constituents in multi-arch retaining structure |
| CN106928376B (en) * | 2017-03-23 | 2019-01-15 | 李春生 | The separation method of skunk bush polysaccharide and its application |
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