CN108426960A - The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid - Google Patents
The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid Download PDFInfo
- Publication number
- CN108426960A CN108426960A CN201810462564.5A CN201810462564A CN108426960A CN 108426960 A CN108426960 A CN 108426960A CN 201810462564 A CN201810462564 A CN 201810462564A CN 108426960 A CN108426960 A CN 108426960A
- Authority
- CN
- China
- Prior art keywords
- acid
- oleanolic acid
- ursolic acid
- reference substance
- sample
- 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
-
- 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
Abstract
The present invention proposes a kind of content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid, and its step are as follows：（1）Common Floweringqince Fruit is taken, is set in conical flask with cover, methanol, close plug, weighed weight is added；It is ultrasonically treated, cooled to room temperature, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, filtering with microporous membrane takes subsequent filtrate as test solution；（2）Using the content of oleanolic acid and ursolic acid in high effective liquid chromatography for measuring test solution, chromatographic condition when measurement is：Chromatographic column is (2) 250 × 4.6mm of Agilent5 TC C18, may be implemented to measure oleanolic acid in Fructus Chaenomelis and ursolic acid content, its separating degree is made to reach qualified.
Description
Technical field
The present invention relates to a kind of assay method, more particularly to a kind of assay side of oleanolic acid in Fructus Chaenomelis and ursolic acid
Method.
Background technology
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) measures horsewhip using Thin-layer scanning chromatography
Ursolic acid content in grass, this method are influenced by factors such as lamellae, temperature, point sample, colour developings, and it is inclined to easily lead to quantitative analysis results
Difference, and can not Accurate Determining go out the content of another active ingredient-oleanolic acid.
Chinese medicine pawpaw is in checkout procedure, and discovery is when assay is examined, the detection side according to Chinese Pharmacopoeia one
The separating degree of method oleanolic acid and ursolic acid is not achieved 1.5 or more at all, makes assay that can not carry out, and makes the quality control of pawpaw
System can not be solved from basic；In view of the consideration to drug quality safety, it is necessary to invent new method.
Invention content
In view of the above-mentioned problems, the present invention proposes a kind of content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid, it can
Oleanolic acid in Fructus Chaenomelis and ursolic acid content are measured with realizing, its separating degree is made to reach qualified.
Specific technical solution is as follows：
The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid, its step are as follows：
（1）Common Floweringqince Fruit is taken, is set in conical flask with cover, methanol, close plug, weighed weight is added；It is ultrasonically treated, naturally cools to room
Temperature, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, and filtering with microporous membrane takes subsequent filtrate as test solution；
（2）Using the content of oleanolic acid and ursolic acid in high effective liquid chromatography for measuring test solution, chromatography when measurement
Condition is：Chromatographic column is (2) 250 × 4.6mm of Agilent5 TC-C18.
Further, when measurement, mobile phase is (methanol：Water：Phosphoric acid (90:10:0.05)〕:Water (90:10) solution, column
17 DEG C, Detection wavelength 210mm, flow velocity 0.8ml/min of temperature.
Further, step（1）In Common Floweringqince Fruit in the sieve of weighed preceding mistake four.
Further, specific experimental method is as follows for assay：
（1）The preparation of reference substance stock solution：Precision weighs oleanolic acid reference substance 5.53mg, ursolic acid reference substance 6.24mg respectively
It sets in 50ml measuring bottles, respectively plus methanol dissolves and be diluted to 50ml, as a contrast product stock solution；
（2）The preparation of test solution：Common Floweringqince Fruit 0.5g is taken, it is accurately weighed, it sets in conical flask with cover, methanol is added in precision
25ml, close plug, weighed weight；After being ultrasonically treated 30 minutes, cooled to room temperature, then weighed weight, supply less loss with methanol
Weight, shake up, filtering with microporous membrane takes subsequent filtrate as test solution；
（3）Linear relationship is investigated：Each 0.5ml, 1.0ml of reference substance stock solution of precision absorption oleanolic acid and ursolic acid,
2.0ml, 3.0ml, 4.0ml are set in 10ml measuring bottles, and mobile phase is added to be diluted to scale, are shaken up, and the reference substance for obtaining various concentration is molten
Liquid；Precision draws each 10ul of above-mentioned 5 kinds of reference substance solutions and distinguishes sample introduction by chromatographic condition, measures；With reference substance concentration X（ug/
ml）For abscissa, peak area Y is that ordinate carries out linear regression, obtains regression equation；Oleanolic acid:Y=37.51X-19.72(r=
0.9997), range of linearity 5.23691-40.56808ug/ml；Ursolic acid:Y=12.38X-24.52 (r=0.9999), line
Property ranging from 5.90928-47.27424ug/ml；The result shows that oleanolic acid and ursolic acid are respectively within the scope of corresponding sample size
With good linear relationship；
（4）Repeated experiment：It takes and step（2）Step is pressed with batch of sample（2）Prepare and sample introduction measure, oleanolic acid and
The RSD of ursolic acid content is respectively 1.02% and 1.05%, shows that this method is reproducible；
（5）Stability experiment：Take step（4）The same batch of sample prepared was measured in 4 hours, 8 hours, 12 hours difference sample introductions,
As a result the chromatographic peak area of oleanolic acid and ursolic acid is respectively 0.35% and 0.42% without significant change, RSD in 12 hours, is shown
Sample is good in 12 hours internal stabilities；
（6）Precision Experiment：Precision draws reference substance solution in continuous sample introduction 6 times, as a result oleanolic acid and ursolic acid heavy colour spectrum
Peak area RSD is respectively 0.32% and 0.30%, shows that this method precision is good；
（7）Sample recovery rate is tested：It is respectively that 0.909% and 0.161% sample 0.50g is total to take oleanolic acid and ursolic acid content
6 parts, it is separately added into reference substance storing solution 1.0ml, 2.0ml, 3.0ml, method prepares test solution, is measured, calculates back
Yield；
（8）The pawpaw sample of different batches is taken to be prepared by test solution the preparation method respectively, traveling sample of going forward side by side measures, theoretical plate
Number and separating degree can reach the standard of Chinese Pharmacopoeia.
Further, step（1）In oleanolic acid reference substance be purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:
110709-201607, purity 91.7%；Ursolic acid reference substance is purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:110742-
201622, purity 94.7%；Methanol is chromatographically pure；Water is Wahaha Pure Water, remaining reagent is that analysis is pure.
Further, step（2）In supersound process power be 250W, frequency 40KHZ.
Beneficial effects of the present invention are：
The oleanolic acid and ursolic acid contained in pawpaw has anticancer, improves immunity, reducing blood lipid and hypoglycemic and other effects, pawpaw
The method of oleanolic acid and ursolic acid content in medicinal material provides foundation for the quality control of pawpaw.
This method may be implemented to measure oleanolic acid in Fructus Chaenomelis and ursolic acid content, it can make the chromatographic peak separation of the two
Degree reaches 1.5 or more, and number of theoretical plate is not less than 5000 based on oleanolic acid peak, and the method for the present invention is simple, easy to operation, safely may be used
It leans on.
Specific implementation mode
It is clear to make technical scheme of the present invention be more clear, below the present invention is described further, it is any to this
The technical characteristic of inventive technique scheme carries out the scheme that equivalencing is obtained with conventional reasoning and each falls within the scope of the present invention.
The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid, its step are as follows：
（1）Common Floweringqince Fruit 0.5g is taken, it is accurately weighed, it sets in conical flask with cover, methanol 25ml, close plug, weighed weight is added in precision；
After being ultrasonically treated 30 minutes, cooled to room temperature, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, miillpore filter
Filtering, takes subsequent filtrate as test solution；
（2）Using the content of oleanolic acid and ursolic acid in high effective liquid chromatography for measuring test solution, chromatography when measurement
Condition is：Chromatographic column is (2) 250 × 4.6mm of Agilent5 TC-C18.
Further, when measurement, mobile phase is (methanol：Water：Phosphoric acid (90:10:0.05)〕:Water (90:10) solution, column
17 DEG C, Detection wavelength 210mm, flow velocity 0.8ml/min of temperature.
Further, step（1）In Common Floweringqince Fruit in the sieve of weighed preceding mistake four.
Further, specific experimental method is as follows for assay：
（1）The preparation of reference substance stock solution：Precision weighs oleanolic acid reference substance 5.53mg, ursolic acid reference substance 6.24mg respectively
It sets in 50ml measuring bottles, respectively plus methanol dissolves and be diluted to 50ml, as a contrast product stock solution；
（2）The preparation of test solution：Common Floweringqince Fruit 0.5g is taken, it is accurately weighed, it sets in conical flask with cover, methanol is added in precision
25ml, close plug, weighed weight；After being ultrasonically treated 30 minutes, cooled to room temperature, then weighed weight, supply less loss with methanol
Weight, shake up, filtering with microporous membrane takes subsequent filtrate as test solution；
（3）Linear relationship is investigated：Each 0.5ml, 1.0ml of reference substance stock solution of precision absorption oleanolic acid and ursolic acid,
2.0ml, 3.0ml, 4.0ml are set in 10ml measuring bottles, and mobile phase is added to be diluted to scale, are shaken up, and the reference substance for obtaining various concentration is molten
Liquid；Precision draws each 10ul of above-mentioned 5 kinds of reference substance solutions and distinguishes sample introduction by chromatographic condition, measures；With reference substance concentration X（ug/
ml）For abscissa, peak area Y is that ordinate carries out linear regression, obtains regression equation；Oleanolic acid:Y=37.51X-19.72(r=
0.9997), range of linearity 5.23691-40.56808ug/ml；Ursolic acid:Y=12.38X-24.52 (r=0.9999), line
Property ranging from 5.90928-47.27424ug/ml；The result shows that oleanolic acid and ursolic acid are respectively within the scope of corresponding sample size
With good linear relationship；
（4）Repeated experiment：It takes and step（2）Step is pressed with batch of sample（2）Prepare and sample introduction measure, oleanolic acid and
The RSD of ursolic acid content is respectively 1.02% and 1.05%, shows that this method is reproducible；
（5）Stability experiment：Take step（4）The same batch of sample prepared was measured in 4 hours, 8 hours, 12 hours difference sample introductions,
As a result the chromatographic peak area of oleanolic acid and ursolic acid is respectively 0.35% and 0.42% without significant change, RSD in 12 hours, is shown
Sample is good in 12 hours internal stabilities；
（6）Precision Experiment：Precision draws reference substance solution in continuous sample introduction 6 times, as a result oleanolic acid and ursolic acid heavy colour spectrum
Peak area RSD is respectively 0.32% and 0.30%, shows that this method precision is good；
（7）Sample recovery rate is tested：It is respectively that 0.909% and 0.161% sample 0.50g is total to take oleanolic acid and ursolic acid content
6 parts, it is separately added into reference substance storing solution 1.0ml, 2.0ml, 3.0ml, method prepares test solution, is measured, calculates back
The experimental result of yield, sample recovery rate is as shown in table 1；
（8）The pawpaw sample of different batches is taken to be prepared by test solution the preparation method respectively, traveling sample of going forward side by side measures, theoretical plate
Number and separating degree can reach the standard of Chinese Pharmacopoeia.
Further, step（1）In oleanolic acid reference substance be purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:
110709-201607, purity 91.7%；Ursolic acid reference substance is purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:110742-
201622, purity 94.7%；Methanol is chromatographically pure；Water is Wahaha Pure Water, remaining reagent is that analysis is pure.
Further, step（2）In supersound process power be 250W, frequency 40KHZ.
Table 1：Sample recovery rate experimental result
Claims (6)
1. the content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid, it is characterized in that, its step are as follows：
（1）Common Floweringqince Fruit is taken, is set in conical flask with cover, methanol, close plug, weighed weight is added；It is ultrasonically treated, naturally cools to room
Temperature, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, and filtering with microporous membrane takes subsequent filtrate as test solution；
（2）Using the content of oleanolic acid and ursolic acid in high effective liquid chromatography for measuring test solution, chromatography when measurement
Condition is：Chromatographic column is (2) 250 × 4.6mm of Agilent5 TC-C18.
2. the content assaying method of oleanolic acid in Fructus Chaenomelis as described in claim 1 and ursolic acid, it is characterized in that, when measurement,
Mobile phase is (methanol：Water：Phosphoric acid (90:10:0.05)〕:Water (90:10) solution, 17 DEG C, Detection wavelength 210mm of column temperature, flow velocity
0.8ml/min。
3. the content assaying method of oleanolic acid in Fructus Chaenomelis as described in claim 1 and ursolic acid, it is characterized in that, step（1）
In Common Floweringqince Fruit in the sieve of weighed preceding mistake four.
4. the content assaying method of oleanolic acid in Fructus Chaenomelis as described in claim 1 and ursolic acid, it is characterized in that, assay
Specific experimental method is as follows：
（1）The preparation of reference substance stock solution：Precision weighs oleanolic acid reference substance 5.53mg, ursolic acid reference substance 6.24mg respectively
It sets in 50ml measuring bottles, respectively plus methanol dissolves and be diluted to 50ml, as a contrast product stock solution；
（2）The preparation of test solution：Common Floweringqince Fruit 0.5g is taken, it is accurately weighed, it sets in conical flask with cover, methanol is added in precision
25ml, close plug, weighed weight；After being ultrasonically treated 30 minutes, cooled to room temperature, then weighed weight, supply less loss with methanol
Weight, shake up, filtering with microporous membrane takes subsequent filtrate as test solution；
（3）Linear relationship is investigated：Each 0.5ml, 1.0ml of reference substance stock solution of precision absorption oleanolic acid and ursolic acid,
2.0ml, 3.0ml, 4.0ml are set in 10ml measuring bottles, and mobile phase is added to be diluted to scale, are shaken up, and the reference substance for obtaining various concentration is molten
Liquid；Precision draws each 10ul of above-mentioned 5 kinds of reference substance solutions and distinguishes sample introduction by chromatographic condition, measures；With reference substance concentration X（ug/
ml）For abscissa, peak area Y is that ordinate carries out linear regression, obtains regression equation；Oleanolic acid:Y=37.51X-19.72(r=
0.9997), range of linearity 5.23691-40.56808ug/ml；Ursolic acid:Y=12.38X-24.52 (r=0.9999), line
Property ranging from 5.90928-47.27424ug/ml；The result shows that oleanolic acid and ursolic acid are respectively within the scope of corresponding sample size
With good linear relationship；
（4）Repeated experiment：It takes and step（2）Step is pressed with batch of sample（2）Prepare and sample introduction measure, oleanolic acid and
The RSD of ursolic acid content is respectively 1.02% and 1.05%, shows that this method is reproducible；
（5）Stability experiment：Take step（4）The same batch of sample prepared was measured in 4 hours, 8 hours, 12 hours difference sample introductions,
As a result the chromatographic peak area of oleanolic acid and ursolic acid is respectively 0.35% and 0.42% without significant change, RSD in 12 hours, is shown
Sample is good in 12 hours internal stabilities；
（6）Precision Experiment：Precision draws reference substance solution in continuous sample introduction 6 times, as a result oleanolic acid and ursolic acid heavy colour spectrum
Peak area RSD is respectively 0.32% and 0.30%, shows that this method precision is good；
（7）Sample recovery rate is tested：It is respectively that 0.909% and 0.161% sample 0.50g is total to take oleanolic acid and ursolic acid content
6 parts, it is separately added into reference substance storing solution 1.0ml, 2.0ml, 3.0ml, method prepares test solution, is measured, calculates back
Yield；
（8）The pawpaw sample of different batches is taken to be prepared by test solution the preparation method respectively, traveling sample of going forward side by side measures, theoretical plate
Number and separating degree can reach the standard of Chinese Pharmacopoeia.
5. the content assaying method of oleanolic acid in Fructus Chaenomelis as claimed in claim 4 and ursolic acid, it is characterized in that, step（1）
In oleanolic acid reference substance be purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:110709-201607, purity 91.7%；Bear
Tartaric acid reference substance is purchased from：Nat'l Pharmaceutical ＆ Biological Products Control Institute, lot number:110742-201622, purity 94.7%；Methanol is chromatography
It is pure；Water is Wahaha Pure Water, remaining reagent is that analysis is pure.
6. the content assaying method of oleanolic acid in Fructus Chaenomelis as claimed in claim 4 and ursolic acid, it is characterized in that, step（2）
In supersound process power be 250W, frequency 40KHZ.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810462564.5A CN108426960A (en) | 2018-05-15 | 2018-05-15 | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810462564.5A CN108426960A (en) | 2018-05-15 | 2018-05-15 | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108426960A true CN108426960A (en) | 2018-08-21 |
Family
ID=63163223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810462564.5A Pending CN108426960A (en) | 2018-05-15 | 2018-05-15 | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108426960A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696500A (en) * | 2019-01-29 | 2019-04-30 | 中国药科大学 | Using the method and its application of high effective liquid chromatography for measuring target impurity correction factor |
| CN110646538A (en) * | 2019-09-29 | 2020-01-03 | 单莉 | Pawpaw medicinal material quality evaluation method based on HPLC and SPSS analysis technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064583A1 (en) * | 2004-12-17 | 2006-06-22 | Use-Techno Corporation | Terpene, method for determining its blood concentration, and method for analyzing its pharmacokinetics |
| CN103054972A (en) * | 2012-12-20 | 2013-04-24 | 蚌埠丰原涂山制药有限公司 | Method of extracting oleanolic acid and ursolic acid from pawpaw |
| CN103454229A (en) * | 2013-09-25 | 2013-12-18 | 安徽中医药大学 | Method for discriminating proper picking time of chaenomeles speciosa nakai |
| CN104897795A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in walnut oil through high performance liquid chromatography method |
-
2018
- 2018-05-15 CN CN201810462564.5A patent/CN108426960A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064583A1 (en) * | 2004-12-17 | 2006-06-22 | Use-Techno Corporation | Terpene, method for determining its blood concentration, and method for analyzing its pharmacokinetics |
| CN103054972A (en) * | 2012-12-20 | 2013-04-24 | 蚌埠丰原涂山制药有限公司 | Method of extracting oleanolic acid and ursolic acid from pawpaw |
| CN103454229A (en) * | 2013-09-25 | 2013-12-18 | 安徽中医药大学 | Method for discriminating proper picking time of chaenomeles speciosa nakai |
| CN104897795A (en) * | 2015-04-06 | 2015-09-09 | 查孝柱 | Method for determining oleanolic acid content and ursolic acid content in walnut oil through high performance liquid chromatography method |
Non-Patent Citations (4)
| Title |
|---|
| XINSHENG FANG 等: "Optimization of microwave-assisted extraction followed by RP-HPLC for the simultaneous determination of oleanolic acid and ursolic acid in the fruits of Chaenomeles sinensis", 《J.SEP.SCI.》 * |
| 李晶 等: "木瓜药材HPLC指纹图谱研究", 《植物科学学报》 * |
| 汴京军: "皱皮木瓜皮渣齐墩果酸、熊果酸和总黄酮连续提取工艺研究", 《西南大学学报（自然科学版）》 * |
| 黄浩 等: "高效液相色谱法测定春根藤中的齐墩果酸和熊果酸", 《光谱实验室》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696500A (en) * | 2019-01-29 | 2019-04-30 | 中国药科大学 | Using the method and its application of high effective liquid chromatography for measuring target impurity correction factor |
| CN110646538A (en) * | 2019-09-29 | 2020-01-03 | 单莉 | Pawpaw medicinal material quality evaluation method based on HPLC and SPSS analysis technology |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108426956A (en) | A kind of method of impurity F in Captopril by HPLC | |
| CN108426960A (en) | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid | |
| CN109959735A (en) | The content assaying method of three kinds of ingredients in line leaf broom top, line leaf goldspink flower extract and line leaf goldspink jasmine tea | |
| CN108152399B (en) | Construction and detection method of UPLC (ultra performance liquid chromatography) characteristic spectrum of semen boitae medicinal material | |
| CN109632997A (en) | The extraction and measuring method of regallity glycosides B in a kind of lily medicinal material | |
| CN112730674B (en) | Quality detection method of momordica grosvenori tea | |
| CN106706835A (en) | Quality detection method of trollius chinensis bunge effervescent tablets | |
| CN110441445A (en) | A kind of construction method and flavones ingredient assay of cockscomb HPLC characteristic fingerprint pattern | |
| CN103575823B (en) | The detection method of 8 kinds of chemical compositions in a kind of Tangminling preparation | |
| CN110286169A (en) | A kind of method and its application for extracting and purify respectively 5 kinds of chemical components simultaneously from processing ramulus mori | |
| CN111983120B (en) | Method for establishing characteristic map of wind-dispelling pill mother and measuring content of 7 nucleoside components | |
| CN109856280A (en) | Method that is a kind of while measuring tetrandrine and fangchinoline content in root of fangji medicinal material | |
| CN112051352B (en) | New method for controlling quality of Fukean tablets | |
| CN107941948A (en) | The method that mountain green tea decompression capsule Content of Chlorogenic Acid and rutin detect at the same time | |
| CN111239319A (en) | Method for measuring content of panax japonicus saponin IVa in laryngopharynx clearing oral liquid | |
| CN101153864A (en) | Method for detecting active ingredient content of Yushangling capsules | |
| CN110687224A (en) | Method for measuring triptolide A in tripterygium wilfordii medicinal material and tripterygium wilfordii multi-glycoside tablet prepared from tripterygium wilfordii medicinal material | |
| CN105301122A (en) | Method for determination of contents of oleanolic acid and ursolic acid in kiwi fruit oil through high performance liquid chromatography | |
| CN110568109A (en) | Method for screening radix peucedani feeding materials in lung ventilating and regulating preparation by adopting HPLC (high performance liquid chromatography) | |
| CN110412162A (en) | The quality determining method of the construction method of the HPLC characteristic spectrum of white perfume capsule and white fragrant capsule | |
| CN107356687A (en) | A kind of detection method of alanyl tyrosine content | |
| CN112326806B (en) | Albizzia julibrissin formula particle HPLC characteristic spectrum and construction method and application thereof | |
| CN104546727B (en) | A kind of quinocetone soluble powder and preparation method | |
| CN107037168A (en) | A kind of quality determining method of the brave fruit Chinese herbal granules of the rock of Sugarless type two | |
| CN106177119A (en) | A kind of Fructus Schisandrae Chinensis granule and preparation method thereof |
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: 20180821 |
|
| RJ01 | Rejection of invention patent application after publication |