CN107219315A - A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis - Google Patents
A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis Download PDFInfo
- Publication number
- CN107219315A CN107219315A CN201710212004.XA CN201710212004A CN107219315A CN 107219315 A CN107219315 A CN 107219315A CN 201710212004 A CN201710212004 A CN 201710212004A CN 107219315 A CN107219315 A CN 107219315A
- Authority
- CN
- China
- Prior art keywords
- ase
- verbena officinalis
- hplc methods
- acid
- methanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis, belong to field of chemical detection.Aiming to provide one kind can be while determines oleanolic acid and ursolic acid content in Verbena officinalis, and easy to operate, sensitivity is high, the ASE HPLC methods that have good stability.This method is extracted using ASE methods with methanol to the Verbena officinalis after crushing, collects methanol extraction liquid；The content of oleanolic acid and ursolic acid in Verbena officinalis is determined using HPLC methods, wherein chromatographic column used is Thermo Acclaim C30.The present invention can be used for the quality control and evaluation of Verbena officinalis.
Description
Technical field
The invention belongs to field of chemical detection, especially a kind of ASE-HPLC methods determine oleanolic acid and black bearberry in Verbena officinalis
The method of acid content.
Background technology
Verbena officinalis is the dry aerial parts of Verbenaceae.Its is cool in nature, bitter, nontoxic；With clearing heat and detoxicating, blood-breaking
Stimulate the menstrual flow, effect of promoting blood circulation to remove blood stasis, inducing diuresis to remove edema.Research shows that Verbena officinalis has obvious anti-inflammatory, Robust speaker feature and anti-human chorionic cancer
Effect, further research learns that the active ingredient of its anticancer is oleanolic acid and ursolic acid.
Oleanolic acid and ursolic acid are isomer, and structure and properties are extremely similar, in natural plants often altogether
Life is mutually deposited, and separation determination is more difficult.Version in 2005《Chinese Pharmacopoeia》(one) determines horsewhip using Thin-layer scanning chromatography
Ursolic acid content in grass, this method is influenceed by factors such as lamellae, temperature, point sample, colour developings, is easily caused quantitative analysis results inclined
Difference, and can not Accurate Determining go out the content of another active ingredient-oleanolic acid.
The content of the invention
For above-mentioned deficiency, contain the present invention is intended to provide one kind can determine oleanolic acid and ursolic acid in Verbena officinalis simultaneously
Amount, and easy to operate, sensitivity is high, the ASE-HPLC methods that have good stability.
In order to realize above-mentioned technique effect, the technical scheme that the present invention is provided is such：A kind of ASE-HPLC methods are determined
The method of oleanolic acid and ursolic acid total content in Verbena officinalis, comprises the steps successively：
Step 1：The Verbena officinalis after crushing is extracted with methanol using ASE methods, methanol extraction liquid is collected；
Step 2：The content of oleanolic acid and ursolic acid in Verbena officinalis is determined using HPLC methods, wherein chromatographic column used is
Thermo Acclaim C30。
Further, the specification of the chromatographic column described in step 2 is 3 μm, 2.1*150mm.
Further, described step 1 includes following sub-steps：
Step S1：Verbena officinalis sample comminution is crossed into No. three sieves, takes 0.25g to be mixed with 1g diatomite；
Step S2：Step 1 gained mixture is put in the 10mlASE abstraction pools equipped with fibrous filter membrane, plus diatomite to
Pond mouthful is parallel；
Step S3：Extracted with 25ml methanol, with methanol constant volume to 25ml after terminating, obtain methanol extraction liquid.
Further, the extraction described in step S3, parameter is as follows：Extraction temperature is 100 DEG C, and extraction time is 6min, extraction
It is 1 time to take number of times, and pressure is 1500psi, and flush volume is 60%, and purge time is 60s.
Further, the detection parameter of the HPLC methods described in step 2 is as follows：Column temperature is 40 DEG C；Flow velocity is 0.3mL/min；
Mobile phase is the acetic acid of methanol -0.2%；Detection wavelength is 205nm.
Further, the volume ratio of the acetic acid of methanol -0.2% of described mobile phase is 90:10.
Further, instrument used in described ASE methods is the ASE350 Accelerate solvent extractions of DIONEX companies of the U.S.
The instrument that instrument, HPLC methods are used is the high performance liquid chromatograph of Agilent -1290.
The present invention is compared with conventional method, with advantages below：
1. the present invention is once investigated to the solvent that Accelerate solvent extraction is used, there is paper to mention and extracted using 70% ethanol
Oleanolic acid and ursolic acid relative amount are higher, therefore to having carried out solvent investigation using methanol and 70% ethanol and absolute ethyl alcohol,
As a result show that methanol, 70% ethanol are consistent with ursolic acid content with absolute ethyl alcohol extraction oleanolic acid, and impurity peaks are essentially identical,
Therefore Extraction solvent is used as using methanol；
2. the present invention has investigated extraction times to be influenceed on it, sample is taken to carry out extraction 1 time, 2 times, 3 times to it in experiment, point
As a result analysis as a result, show that extraction is once almost complete, therefore experiment uses the method for extraction once；
3. the present invention, which improves temperature, reduces the viscosity of solvent, the prevention that solvent enters sample matrices is reduced, is added
Solvent enters the diffusion of sample matrices, and the surface tension between reduction solvent and sample matrices makes solvent dissolve the appearance of determinand
Amount increase；
4. due to liquid to the solvability of solute much larger than solvability of the gas to solute, therefore the boiling point of extraction liquids
Improved with pressure rise, so that solvent remains at liquid at high temperature under high pressure.
Brief description of the drawings
Fig. 1 is the chromatogram of oleanolic acid reference substance and ursolic acid reference substance mixed liquor；
Fig. 2 is the chromatogram of oleanolic acid and ursolic acid in the sample determined using ASE-HPLC methods；
Fig. 3 is the chromatogram of oleanolic acid and ursolic acid in the sample determined using official method.
Embodiment
With reference to embodiment, the claim to the present invention is described in further detail, but is not constituted pair
Any limitation of the present invention, any limited number of time modification made in the claims in the present invention protection domain, still the present invention's
In claims.
Embodiment 1
1. instrument and equipment and reagent
1.1 instrument：
Electronic analytical balance (XA205DU), ASE350 Accelerate solvent extractions instrument (DIONEX companies of the U.S.), high-efficient liquid phase color
Spectrometer (1290)
1.2 reagents (in addition to especially indicating, this experiment agents useful for same is that analysis is pure)：
Water：Meet one-level water as defined in GB/T 6682；
Methanol (CH4O)：Chromatographically pure (phase chromatography-use)；
Ethanol (C2H5OH)：Analysis is pure.
2 methods
The preparation of 2.1 reference substance solutions：
Take oleanolic acid reference substance, ursolic acid reference substance appropriate, it is accurately weighed, plus every 1ml is made containing oleanolic acid in methanol
50 μ g, ursolic acid 0.1mg mixed solution, are produced.
The preparation of 2.2 need testing solutions
2.2.1《Chinese Pharmacopoeia》Version one prepares test sample method within 2015：
This product powder (crossing No. four sieves) about 0.5g is taken, it is accurately weighed, put in conical flask with cover, precision adds absolute ethyl alcohol
25ml, weighed weight is heated to reflux 4 hours, let cool, then weighed weight, and the weight of less loss is supplied with absolute ethyl alcohol, is shaken up, filter
Cross.Precision measures subsequent filtrate 10ml, plus 1% ammonia spirit 3ml, mixes, and with petroleum ether, (30~60 DEG C) shake extraction 3 times, often
Secondary 15ml, discards petroleum ether liquid, takes ethanol to be evaporated, residue adds methanol to dissolve, and is transferred in 5ml measuring bottles, plus methanol is extremely carved
Degree, shakes up, and filters, takes subsequent filtrate, produce.
2.2.2 Accelerate solvent extraction method (ASE) prepares test sample method：
The size-reduced machine of sample is crushed, and is crossed No. three sieves, is taken 0.25g, accurately weighed, is well mixed with about 1g diatomite, stand-by,
It is moved into the ASE 10ml abstraction pools for putting fibrous filter membrane well in advance and adds appropriate diatomite, gently shaking is allowed to exist with Chi Kou
In same horizontal line, tighten and covered on abstraction pool, be put into rapid extracting device and extracted.After extraction terminates, extract is shifted
Into 25ml volumetric flasks, extraction flask is cleaned with a small amount of methanol and is incorporated into volumetric flask for 3 times, using methanol constant volume to scale, is produced.
2.3ASE extraction conditions
Described extraction, parameter is as follows：Extraction temperature is 100 DEG C, and extraction time is 6min, and extraction times are 1 time, pressure
For 1500psi, flush volume is 60%, and purge time is 60s.
2.4 chromatographic conditions and system suitability
Using octadecylsilane chemically bonded silica as filler；With the acetum of methanol -0.2% (82.5:17.5) it is flowing
Phase；EISD is detected.Number of theoretical plate is calculated by ursolic acid peak should be not less than 5000.
2.5 determination method
Determined according to high performance liquid chromatography (general rule 0512)
It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected, determines, produces.
Detect that parameter is as follows：Instrument：Agilent-high performance liquid chromatograph (1290)；Chromatographic column is Thermo
AcclaimC30,3 μm, 2.1*150mm；Column temperature is 40 DEG C；Flow velocity is 0.3mL/min；Mobile phase is that volume ratio is 90:10
The acetic acid of methanol -0.2%；Detection wavelength is 205nm.
The requirement of 2.6 standard limited values
This product is calculated by dry product, and the total amount containing oleanolic acid (C30H48O3) and ursolic acid (C30H48O3) must not be less than
0.30%.
2.7 calculate (external standard method)
C in formulaR--- reference substance solution concentration, unit is micro- gram per liter (mg/L)；
AX--- the peak area of test sample；
AR--- reference substance peak area.
Note：
It should be dismantled and cleaned out using preceding extraction bottom of pond portion, otherwise easily cause pressure instability；
Otherwise the filter paper of abstraction pool bottom should cause seepage in sealing ring；
Abstraction pool fills elastic moderate during sample, and too loose to be easily caused extract solution excessive；
Check whether gas cylinder air pressure reaches 1Mpa before start；
Using being cleaned out after terminating, abstraction pool will in time dry and (get rusty easily).
3 results
3.1 chromatogram
Fig. 1 is the chromatogram of oleanolic acid reference substance and ursolic acid reference substance mixed liquor；
Fig. 2 is the chromatogram of oleanolic acid and ursolic acid in the sample determined using ASE-HPLC methods；
Fig. 3 is the chromatogram of oleanolic acid and ursolic acid in the sample determined using official method.
Wherein, the retention time of oleanolic acid is that 5.424min, the retention time of ursolic acid are 5.907 in fig. 1-3.
3.2 replica test
Take the sample (lot number of identical lot number：20150801) 0.5g, it is totally 6 parts, accurately weighed, extracted by ASE extracting methods
Need testing solution, sample size is 3 μ L, with above-mentioned chromatographic condition parallel test, measures oleanolic acid and ursolic acid in sample and contains
It is 2.4% that the content of amount, which is shown in Table 1, RSD, and experiment shows that ASE extracting methods repeatability is good.
Table 1
3.3 sample size measurement results (3 batches)
The present invention has used two Accelerate solvent extraction instrument and official method to extract Verbena officinalis sample respectively, extracts
It the results are shown in Table 2：
Table 2
The data comparison that ASE1 extracts oleanolic acid and ursolic acid total content in sample with official method the results are shown in Table 3：
Table 3
| Lot number | ASE1 | Pharmacopeia | Average value | RAD% |
| 15062801 | 0.368 | 0.316 | 0.342 | 7.60 |
| 1507103 | 0.414 | 0.355 | 0.385 | 7.67 |
| 20150801 | 0.400 | 0.343 | 0.372 | 7.67 |
The data comparison that ASE2 extracts oleanolic acid and ursolic acid total content in sample with official method the results are shown in Table 4：
Table 4
| Lot number | ASE2 | Pharmacopeia | Average value | RAD% |
| 15062801 | 0.385 | 0.316 | 0.351 | 9.84 |
| 1507103 | 0.401 | 0.355 | 0.378 | 6.08 |
| 20150801 | 0.382 | 0.343 | 0.363 | 5.38 |
Data comparison between two ASE instruments is shown in Table 5：
Table 5
| Lot number | ASE1 | ASE2 | Average value | RAD% |
| 15062801 | 0.368 | 0.385 | 0.377 | 2.26 |
| 1507103 | 0.414 | 0.401 | 0.408 | 1.60 |
| 20150801 | 0.400 | 0.382 | 0.391 | 2.30 |
4 discuss
The selection of 4.1ASE Extraction solvents：
In experiment, once the solvent that Accelerate solvent extraction is used was investigated, has paper to mention and is extracted using 70% ethanol
Oleanolic acid and ursolic acid relative amount are higher, therefore to having carried out solvent investigation using methanol and 70% ethanol and absolute ethyl alcohol,
As a result show that methanol, 70% ethanol are consistent with ursolic acid content with absolute ethyl alcohol extraction oleanolic acid, and impurity peaks are essentially identical,
Therefore Extraction solvent is used as using methanol.
The optimization of 4.2ASE extraction conditions
On above-mentioned experiment basis, extraction times are mainly investigated in this experiment to be influenceed on it, takes sample to carry out it in experiment
As a result extraction 1 time, 2 times, 3 times, analysis as a result, show that extraction is once almost complete.
Therefore method of the experiment using extraction once.
Claims (7)
1. a kind of method of the oleanolic acid and ursolic acid total content in ASE-HPLC methods measure Verbena officinalis, it is characterised in that according to
It is secondary to comprise the steps：
Step 1：The Verbena officinalis after crushing is extracted with methanol using ASE methods, methanol extraction liquid is collected；
Step 2：The content of oleanolic acid and ursolic acid in Verbena officinalis is determined using HPLC methods, wherein chromatographic column used is Thermo
Acclaim C30。
2. a kind of ASE-HPLC methods according to claim 1 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that the specification of the chromatographic column described in step 2 is 3 μm, 2.1*150mm.
3. a kind of ASE-HPLC methods according to claim 1 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that described step 1 includes following sub-steps：
Step S1：Verbena officinalis sample comminution is crossed into No. three sieves, takes 0.25g to be mixed with 1g diatomite；
Step S2：Step 1 gained mixture is put in the 10mlASE abstraction pools equipped with fibrous filter membrane, plus diatomite to and Chi Kou
It is parallel；
Step S3：Extracted with 25ml methanol, with methanol constant volume to 25ml after terminating, obtain methanol extraction liquid.
4. a kind of ASE-HPLC methods according to claim 3 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that the extraction described in step S3, parameter is as follows：Extraction temperature is 100 DEG C, and extraction time is 6min, extraction
Number of times is 1 time, and pressure is 1500psi, and flush volume is 60%, and purge time is 60s.
5. a kind of ASE-HPLC methods according to claim 1 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that the detection parameter of the HPLC methods described in step 2 is as follows：Column temperature is 40 DEG C；Flow velocity is 0.3mL/min；Stream
Dynamic is mutually the acetic acid of methanol -0.2%；Detection wavelength is 205nm.
6. a kind of ASE-HPLC methods according to claim 5 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that the volume ratio of the acetic acid of methanol -0.2% of described mobile phase is 90:10.
7. a kind of ASE-HPLC methods according to claim 1 determine oleanolic acid in Verbena officinalis and ursolic acid total content
Method, it is characterised in that instrument used in described ASE methods is the ASE350 Accelerate solvent extractions of DIONEX companies of the U.S.
The instrument that instrument, HPLC methods are used is the high performance liquid chromatograph of Agilent -1290.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710212004.XA CN107219315A (en) | 2017-04-01 | 2017-04-01 | A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710212004.XA CN107219315A (en) | 2017-04-01 | 2017-04-01 | A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107219315A true CN107219315A (en) | 2017-09-29 |
Family
ID=59927572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710212004.XA Pending CN107219315A (en) | 2017-04-01 | 2017-04-01 | A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107219315A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610417A (en) * | 2015-02-16 | 2015-05-13 | 白心亮 | Method for extracting ursolic acid and oleanolic acid from hawthorns |
| CN104825577A (en) * | 2015-04-07 | 2015-08-12 | 西南大学 | Method for combined production of oleanolic acid, ursolic acid and general flavones from chaenomeles speciosa peel dregs |
| CN104897798A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in peanut oil through high performance liquid chromatography method |
| CN104897796A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in sesame oil through high performance liquid chromatography method |
| CN105699539A (en) * | 2016-04-15 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for extracting oleanolic acid in clematis root |
-
2017
- 2017-04-01 CN CN201710212004.XA patent/CN107219315A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610417A (en) * | 2015-02-16 | 2015-05-13 | 白心亮 | Method for extracting ursolic acid and oleanolic acid from hawthorns |
| CN104897798A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in peanut oil through high performance liquid chromatography method |
| CN104897796A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in sesame oil through high performance liquid chromatography method |
| CN104825577A (en) * | 2015-04-07 | 2015-08-12 | 西南大学 | Method for combined production of oleanolic acid, ursolic acid and general flavones from chaenomeles speciosa peel dregs |
| CN105699539A (en) * | 2016-04-15 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for extracting oleanolic acid in clematis root |
Non-Patent Citations (2)
| Title |
|---|
| 张晓喻 等: "RP-HPLC测定四川不同产地枇杷花中齐墩果酸和熊果酸的含量", 《药物分析杂志》 * |
| 赵亮: "中药复方清肝散结颗粒的药效物质基础及质量控制研究", 《中国博士学位论文全文数据库 医药卫生科技辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108169356A (en) | A kind of method that ASE-HPLC methods measure spinosin content in spina date seed | |
| CN107064347A (en) | A kind of ASE HPLC methods determine Psoralen, the method for Isopsoralen content in Psoralen ester | |
| CN107219315A (en) | A kind of method that ASE HPLC methods determine oleanolic acid and ursolic acid total content in Verbena officinalis | |
| CN108107129A (en) | A kind of method for measuring ursolic acid total content in Verbena officinalis | |
| CN108020624A (en) | A kind of method for measuring oleanolic acid total content in Verbena officinalis | |
| CN106831914A (en) | A kind of method that ASE methods extract aurantiamarin in dried orange peel | |
| CN106872611A (en) | A kind of method that ASE HPLC methods determine amentoflavone content in Selaginella tamariscina | |
| CN106885860A (en) | A kind of method that ASE HPLC methods determine spinosin content in spina date seed | |
| CN106955502A (en) | A kind of method of Geniposidic acid and acteoside in ASE methods extraction plantain seed | |
| CN108107127A (en) | A kind of method of ginsenoside Re's content in measure ginseng | |
| CN106924990A (en) | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia | |
| CN106885862A (en) | A kind of ASE HPLC methods determine peimine, the method for the content of Peiminine in fritillaria thunbergii | |
| CN108169352A (en) | A kind of method that ASE-HPLC methods measure amentoflavone content in Selaginella tamariscina | |
| CN106885861A (en) | A kind of method that ASE HPLC methods determine isoferulic acid content in rattletop | |
| CN107014927A (en) | A kind of method that ASE HPLC methods determine Determination of hesperidin in pericarpium citri reticulatae | |
| CN108169353A (en) | A kind of method that ASE-HPLC methods measure Determination of hesperidin in pericarpium citri reticulatae | |
| CN108101949A (en) | A kind of method of aurantiamarin in ASE methods extraction dried orange peel | |
| CN106918666A (en) | A kind of method that ASE HPLC methods determine the curculigoside content in thizoma curculiginis | |
| CN107064384A (en) | A kind of method that ASE methods extract spinosin in spina date seed | |
| CN107892706A (en) | A kind of method of spinosin in ASE methods extraction spina date seed | |
| CN108169355A (en) | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia | |
| CN106872610A (en) | A kind of method that ASE HPLC methods determine castor-oil plant alkali content in castor bean | |
| CN107064344A (en) | A kind of method that ASE HPLC methods determine ginsenoside Rg_1 and Re content in ginseng | |
| CN107831256A (en) | A kind of method of Geniposidic acid and acteoside content in ASE HPLC methods measure plantain seed | |
| CN108169349A (en) | A kind of method that ASE-HPLC methods measure the content of Peiminine in fritillaria thunbergii |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170929 |
|
| RJ01 | Rejection of invention patent application after publication |