CN106366149B - The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet - Google Patents
The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet Download PDFInfo
- Publication number
- CN106366149B CN106366149B CN201610647340.2A CN201610647340A CN106366149B CN 106366149 B CN106366149 B CN 106366149B CN 201610647340 A CN201610647340 A CN 201610647340A CN 106366149 B CN106366149 B CN 106366149B
- Authority
- CN
- China
- Prior art keywords
- medroxyprogesterone acetate
- crude product
- volume
- relevant material
- silica gel
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J7/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms
- C07J7/0005—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21
- C07J7/001—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group
- C07J7/004—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group substituted in position 17 alfa
- C07J7/0045—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group substituted in position 17 alfa not substituted in position 16
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses the relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet, preparation method includes：High temperature：Medroxyprogesterone acetate bulk drug is put into 100~120 DEG C to destroy 16~24 hours；Enrichment：High temperature sample is dissolved in 60%~70% methanol aqueous solution, stirred, is filtered, collects filtrate, be concentrated under reduced pressure to obtain concentrate；It is prepared by crude product：Concentrate is separated with normal phase silica gel column chromatography, is concentrated to give crude product；It is refined：Crude product reverse phase silica gel post is purified, stationary phase is octadecylsilane chemically bonded silica, and mobile phase is 65%~75% acetonitrile solution, isocratic elution, collects the 8th~12 column volume eluent, concentration, is freeze-dried and produces.The relevant material can detect the composition, and content is more than 5/10000ths, it is necessary to carry out analysis and Control to it to report first in medroxyprogesterone acetate bulk drug and tablet.
Description
Technical field
The invention belongs to System In Pharmaceutical Preparation Analysis field, and in particular to a kind of relevant material of medroxyprogesterone acetate dispersible tablet and
Its analyzing detecting method.
Background technology
Medroxyprogesterone acetate dispersible tablet, indication are recurrent or metastatic hormone-dependent neoplasm for that can not perform the operation
Palliative treatment or auxiliary treatment, such as carcinoma of endometrium, kidney, breast cancer.
The active component of medroxyprogesterone acetate dispersible tablet is medroxyprogesterone acetate, and medroxyprogesterone acetate is as breast cancer, son
The endocrine therapeutic agents of the hormone-dependent neoplasms such as endometrial carcinoma, and for treat irregular menstruation, functional uterine bleeding,
Endometriosis, also the progestational hormone composition available for short-acting combined oral contraceptive, and being prevented miscarriage available for pregnant woman.Face at present
Bed extensive use simultaneously obtains relatively satisfactory effect.Meanwhile medroxyprogesterone acetate is as endocrine agents are alone or and antineoplastic
Thing shares the effect that treatment prostate cancer, kidney, prostatic adenoma are also improved curative effect.Other treatment breast cancer, endometrium
Cancer, prostate cancer, kidney, the chemotherapeutics of prostatic adenoma have certain toxic side effect, produce injury to patient's body, still
The advantages of medroxyprogesterone acetate, is to be not only able to monotherapy or synergistic treatment, moreover it is possible to is obviously improved apocleisis, the body weight of patient
The symptom such as mitigation and cachexia, so as to improve the overall health of patients of patient and quality of life.
Medroxyprogesterone acetate chemical structural formula is as follows：
The content of the invention
The present invention provides the relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet first.
An object of the present invention is to provide the relevant material in a kind of medroxyprogesterone acetate dispersible tablet, and chemical structural formula is such as
Under：
The second object of the present invention is to provide the above-mentioned preparation method about material, comprises the following steps：
Step S1, high temperature：It is small that 16~24 are destroyed under the conditions of medroxyprogesterone acetate bulk drug is placed in into 100~120 DEG C
When；
Step S2, enrichment：Above-mentioned high temperature sample is dissolved in the methanol that methanol concentration expressed in percentage by volume is 60%~70%
In the aqueous solution, stir, filter, collect filtrate, be concentrated under reduced pressure to obtain concentrate；
It is prepared by step S3, crude product：Above-mentioned concentrate is separated with normal phase silica gel column chromatography, is successively 30 with volume ratio:1、
15:1 and 8:1 methylene chloride-methanol mixed solvent gradient elution, collect 8:1 elution fraction, is concentrated to give crude product；
Step S4, refine：Above-mentioned crude product reverse phase silica gel post to be purified, stationary phase is octadecylsilane chemically bonded silica,
Mobile phase is the acetonitrile solution that acetonitrile concentration expressed in percentage by volume is 65%~75%, isocratic elution, collects the 8th~12 column volume
Eluent, concentration, is freeze-dried and produces the relevant material.
Further, described preparation method comprises the following steps：
Step S1, high temperature：Destroyed 20 hours under the conditions of medroxyprogesterone acetate bulk drug is placed in into 110 DEG C；
Step S2, enrichment：Above-mentioned high temperature sample is dissolved in the methanol aqueous solution that methanol concentration expressed in percentage by volume is 65%
In, stir, filter, collect filtrate, be concentrated under reduced pressure to obtain concentrate；
It is prepared by step S3, crude product：Above-mentioned concentrate is separated with normal phase silica gel column chromatography, is successively 30 with volume ratio:1、
15:1 and 8:1 methylene chloride-methanol mixed solvent gradient elution, collect 8:1 elution fraction, is concentrated to give crude product；
Step S4, refine：Above-mentioned crude product reverse phase silica gel post to be purified, stationary phase is octadecylsilane chemically bonded silica,
Mobile phase is the acetonitrile solution that acetonitrile concentration expressed in percentage by volume is 70%, isocratic elution, collects the 9th~11 column volume elution
Liquid, concentration, is freeze-dried and produces the relevant material.
The third object of the present invention is to provide the above-mentioned analysis method about material, including following parameter：
Chromatographic column：Xtimate C18 (4.6mm × 250mm, 5 μm)；
Mobile phase：A is acetonitrile, and B is the aqueous solution (phosphorus acid for adjusting pH value to 2.8) of the sodium dihydrogen phosphate containing 0.03mol/L；
Gradient elution program：0~6min, A 30%；6~26min, A 30% → 80%；26~32min, A 80%；32
~35min, A 80% → 30%；35~40min, A30%；
Flow rate of mobile phase：1.0mL·min-1；
Detection wavelength：240nm；
Column temperature：35℃；
Sample size：10μL.
The fourth object of the present invention is to provide above-mentioned relevant material in medroxyprogesterone acetate dispersible tablet Related substances separation
Purposes as reference substance.
Advantages of the present invention：
The relevant material is that inventor studies favorite outgoing in the relevant material of medroxyprogesterone acetate dispersible tablet to report first
Now and through structural identification, it is detectable in medroxyprogesterone acetate bulk drug and tablet, and content is more than 5/10000ths, has
Necessity carries out analysis and Control to it.The chromatogram retention behavior about material and medroxyprogesterone acetate is very close, and tradition is isocratic
Chromatographic condition is difficult that analysis finds the presence about material, and therefore, present invention also offers the analysis detection about material
Method.The present invention contributes to the further research that the quality research of medroxyprogesterone acetate dispersible tablet controls, as long-time stability are examined
Examine and investigated with toxicity, to improve the quality standard of medroxyprogesterone acetate dispersible tablet.
Brief description of the drawings
Fig. 1 is the relevant material hydrogen modal data ownership figure of the present invention；
Fig. 2 is the relevant material carbon modal data ownership figure of the present invention.
Embodiment
The essentiality content of the present invention is further illustrated with reference to embodiment, but present invention protection model is not limited with this
Enclose.Although being explained in detail with reference to preferred embodiment to the present invention, it will be understood by those within the art that, can be right
Technical scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention.
Embodiment 1：Preparation and structural identification about material
Take 10g medroxyprogesterone acetate raw materials to be uniformly spread out in culture dish, be placed in baking oven, 110 DEG C are destroyed 20 hours.So
Afterwards, high temperature sample is dissolved in the methanol-water solution that methanol concentration expressed in percentage by volume is 65%, stirred 20 minutes, with suction filtration
Funnel filters, and collects filtrate, be concentrated under reduced pressure to obtain concentrate 6.2g；Then concentrate 10ml methanol is dissolved, is with 15g granularities
The purification on normal-phase silica gel of 100~200 mesh mixes sample, volatilizes solvent, and divided silicon is used as the purification on normal-phase silica gel of 200~300 mesh by the use of 150g granularities
Glue carries out pillar layer separation, is successively 30 with volume ratio:1、15:1 and 8:1 methylene chloride-methanol mixed solvent gradient elution,
Each ratio elutes 10 column volumes, collects 8:1 elution fraction, be concentrated under reduced pressure to obtain crude product 4.1g；Then by crude product acetonitrile body
The acetonitrile solution that product percentage concentration is 70% dissolves, and is purified with reverse phase silica gel post, stationary phase is octadecylsilane bonded silica
Glue, mobile phase are the acetonitrile-water that acetonitrile concentration expressed in percentage by volume is 70%, isocratic elution, collect the elution of the 9th~11 column volume
Liquid, it is concentrated under reduced pressure, is freeze-dried to obtain powder 2.1g.HPLC normalization purity is more than 98%.
Structural identification：
HR-ESIMS is shown [M+H]+For m/z 385.2408, it is C that can obtain molecular formula with reference to nuclear-magnetism feature24H32O4.Hydrogen is composed
Data and ownership are shown in Fig. 1 (ppm, methanol-d4,500MHz)；Carbon modal data and ownership are shown in Fig. 2 (ppm, methanol-d4,
150MHz).Composite mass spectrum and nuclear magnetic data, the chemistry knot of the material can be confirmed with reference to the structural identification data of medroxyprogesterone acetate
Structure formula is as follows：
Embodiment 2：Preparation about material
Take 10g medroxyprogesterone acetate raw materials to be uniformly spread out in culture dish, be placed in baking oven, 100 DEG C are destroyed 24 hours.So
Afterwards, high temperature sample is dissolved in the methanol-water solution that methanol concentration expressed in percentage by volume is 60%, stirred 20 minutes, with suction filtration
Funnel filters, and collects filtrate, be concentrated under reduced pressure to obtain concentrate 6.0g；Then concentrate 10ml methanol is dissolved, is with 15g granularities
The purification on normal-phase silica gel of 100~200 mesh mixes sample, volatilizes solvent, and divided silicon is used as the purification on normal-phase silica gel of 200~300 mesh by the use of 150g granularities
Glue carries out pillar layer separation, is successively 30 with volume ratio:1、15:1 and 8:1 methylene chloride-methanol mixed solvent gradient elution,
Each ratio elutes 10 column volumes, collects 8:1 elution fraction, be concentrated under reduced pressure to obtain crude product 4.0g；Then by crude product acetonitrile body
The acetonitrile solution that product percentage concentration is 65% dissolves, and is purified with reverse phase silica gel post, stationary phase is octadecylsilane bonded silica
Glue, mobile phase are the acetonitrile-water that acetonitrile concentration expressed in percentage by volume is 65%, isocratic elution, collect washing for the 10th~12 column volume
De- liquid, is concentrated under reduced pressure, is freeze-dried to obtain powder 1.9g.HPLC normalization purity is more than 98%.
Embodiment 3：Preparation about material
Take 10g medroxyprogesterone acetate raw materials to be uniformly spread out in culture dish, be placed in baking oven, 120 DEG C are destroyed 16 hours.So
Afterwards, high temperature sample is dissolved in the methanol-water solution that methanol concentration expressed in percentage by volume is 70%, stirred 20 minutes, with suction filtration
Funnel filters, and collects filtrate, be concentrated under reduced pressure to obtain concentrate 6.3g；Then concentrate 10ml methanol is dissolved, is with 15g granularities
The purification on normal-phase silica gel of 100~200 mesh mixes sample, volatilizes solvent, and divided silicon is used as the purification on normal-phase silica gel of 200~300 mesh by the use of 150g granularities
Glue carries out pillar layer separation, is successively 30 with volume ratio:1、15:1 and 8:1 methylene chloride-methanol mixed solvent gradient elution,
Each ratio elutes 10 column volumes, collects 8:1 elution fraction, be concentrated under reduced pressure to obtain crude product 4.2g；Then by crude product acetonitrile body
The acetonitrile solution that product percentage concentration is 75% dissolves, and is purified with reverse phase silica gel post, stationary phase is octadecylsilane bonded silica
Glue, mobile phase are the acetonitrile-water that acetonitrile concentration expressed in percentage by volume is 75%, isocratic elution, collect the elution of the 8th~10 column volume
Liquid, it is concentrated under reduced pressure, is freeze-dried to obtain powder 2.2g.HPLC normalization purity is more than 98%.
Embodiment 4：Medroxyprogesterone acetate dispersible tablet accelerated test (under the conditions of 40 DEG C 30 days) sample detection is analyzed
Medroxyprogesterone acetate dispersible tablet：Collect the medroxyprogesterone acetate dispersible tablet (3 away from the date of manufacture of commercially available different brands
In month).
It is prepared by reference substance solution：Precision weighs the relevant material of the 2mg present invention in 200ml volumetric flasks, and it is fixed to be dissolved with acetonitrile
Hold, as relevant reserve supply liquid；Precision measures relevant reserve supply liquid 1ml in 20ml volumetric flasks, uses liquid phase analysis method
The flowing phase dilution constant volume (about 0.5 μ g/mL) of middle initial proportion.
It is prepared by need testing solution：The medroxyprogesterone acetate dispersible tablet placed 30 days under the conditions of 40 DEG C is taken to be ground into fine powder, essence
The close fine powder that weighs is placed in 25ml volumetric flasks (containing about medroxyprogesterone acetate 12.5mg) in right amount, is added initial in liquid phase analysis method
The mobile phase of ratio, ultrasound dissolve medroxyprogesterone acetate, let cool, and are diluted to scale.
Contrast solution：Precision measures need testing solution 0.5ml in 200ml volumetric flasks, with initial in liquid phase analysis method
The mobile phase of ratio is diluted to scale.
Liquid phase chromatogram condition：
High performance liquid chromatograph：Agilent 1260, binary pump, VWD；
Chromatographic column：Xtimate C18 (4.6mm × 250mm, 5 μm)；
Mobile phase：A is acetonitrile, and B is the aqueous solution (phosphorus acid for adjusting pH value to 2.8) of the sodium dihydrogen phosphate containing 0.03mol/L；
Gradient elution program：0~6min, A 30%；6~26min, A 30% → 80%；26~32min, A80%；32
~35min, A80% → 30%；35~40min, A 30%；
Flow rate of mobile phase：1.0mL·min-1；
Detection wavelength：240nm；
Column temperature：35℃；
Sample size：10μL.
Precision measures relevant material reference substance solution, need testing solution and the μ L of contrast solution 10 injection liquid chromatographs respectively
Analysis.As a result in the medroxyprogesterone acetate dispersible tablet (lot number of Beijing Jiade pharmaceutical Co. Ltd production：And Zhejiang 20150403)
Medroxyprogesterone acetate dispersible tablet (the lot number of Xian Ju Pharmacy stock Co., Ltd production：20150108) detect that the present invention carries in
The relevant material (retention time is 1.25 times of medroxyprogesterone acetate retention time) supplied, the chromatographic peak and tumer about material
Hydroxyprogesterone chromatographic peak separating degree is more than 2.0, and Peak homogeneity is qualified.This in different brands medroxyprogesterone acetate dispersible tablet is relevant
The content of material is 0.05~0.15%, it is necessary to is included in the quality research control of medroxyprogesterone acetate dispersible tablet and enters traveling one
Step research, investigates such as long-time stability and is investigated with toxicity, to improve the quality standard of medroxyprogesterone acetate dispersible tablet.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but the protection of the present invention is not limited with this
Scope.It will be understood by those within the art that technical scheme can be modified or equivalent substitution,
Without departing from the essence and protection domain of technical solution of the present invention.
Claims (4)
1. a kind of preparation method of the relevant material in medroxyprogesterone acetate dispersible tablet, the chemical structural formula about material is such as
Under：
It is characterised in that it includes following steps：
Step S1, high temperature：Destroyed 16~24 hours under the conditions of medroxyprogesterone acetate bulk drug is placed in into 100~120 DEG C；
Step S2, enrichment：It is water-soluble that above-mentioned high temperature sample is dissolved in the methanol that methanol concentration expressed in percentage by volume is 60%~70%
In liquid, stir, filter, collect filtrate, be concentrated under reduced pressure to obtain concentrate；
It is prepared by step S3, crude product：Above-mentioned concentrate is separated with normal phase silica gel column chromatography, is successively 30 with volume ratio:1、15:1
With 8:1 methylene chloride-methanol mixed solvent gradient elution, collect 8:1 elution fraction, is concentrated to give crude product；
Step S4, refine：Above-mentioned crude product reverse phase silica gel post is purified, stationary phase is octadecylsilane chemically bonded silica, flowing
It is mutually the acetonitrile solution that acetonitrile concentration expressed in percentage by volume is 65%~75%, isocratic elution, collects the 8th~12 column volume elution
Liquid, concentration, is freeze-dried and produces the relevant material.
2. preparation method according to claim 1, it is characterised in that comprise the following steps：
Step S1, high temperature：Destroyed 20 hours under the conditions of medroxyprogesterone acetate bulk drug is placed in into 110 DEG C；
Step S2, enrichment：Above-mentioned high temperature sample is dissolved in the methanol aqueous solution that methanol concentration expressed in percentage by volume is 65%, stirred
Mix, filter, collect filtrate, be concentrated under reduced pressure to obtain concentrate；
It is prepared by step S3, crude product：Above-mentioned concentrate is separated with normal phase silica gel column chromatography, is successively 30 with volume ratio:1、15:1
With 8:1 methylene chloride-methanol mixed solvent gradient elution, collect 8:1 elution fraction, is concentrated to give crude product；
Step S4, refine：Above-mentioned crude product reverse phase silica gel post is purified, stationary phase is octadecylsilane chemically bonded silica, flowing
It is mutually the acetonitrile solution that acetonitrile concentration expressed in percentage by volume is 70%, isocratic elution, collects the 9th~11 column volume eluent, it is dense
Contracting, is freeze-dried and produces the relevant material.
3. the analysis method of the relevant material prepared by a kind of claim 1, it is characterised in that including following parameter：
Chromatographic column：Xtimate C18,4.6mm × 250mm, 5 μm；
Mobile phase：A is acetonitrile, and B is the aqueous solution of the sodium dihydrogen phosphate containing 0.03mol/L, phosphorus acid for adjusting pH value to 2.8；
Gradient elution program：0~6min, A 30%；6~26min, A 30% → 80%；26~32min, A 80%；32~
35min, A 80% → 30%；35~40min, A 30%；
Flow rate of mobile phase：1.0mL·min-1；
Detection wavelength：240nm；
Column temperature：35℃；
Sample size：10μL.
4. the relevant material prepared by claim 1 is used as reference substance in medroxyprogesterone acetate dispersible tablet Related substances separation
Purposes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610647340.2A CN106366149B (en) | 2016-08-09 | 2016-08-09 | The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610647340.2A CN106366149B (en) | 2016-08-09 | 2016-08-09 | The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106366149A CN106366149A (en) | 2017-02-01 |
| CN106366149B true CN106366149B (en) | 2018-01-23 |
Family
ID=57878613
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610647340.2A Active CN106366149B (en) | 2016-08-09 | 2016-08-09 | The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106366149B (en) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8362286B2 (en) * | 2009-08-13 | 2013-01-29 | Marinus Pharmaceuticals, Inc. | Method for making 3α-hydroxy, 3β- substituted-5α-pregnan-20-ones |
| CN104231025B (en) * | 2014-09-30 | 2017-12-22 | 华润紫竹药业有限公司 | A kind of estrone bulk drug impurity and preparation method thereof and the purposes as standard items |
| CN105693808B (en) * | 2015-11-05 | 2018-03-16 | 华润紫竹药业有限公司 | A kind of acetic acid crow founds appropriate bulk drug impurity and preparation method thereof and the purposes as standard items |
| CN105669810B (en) * | 2016-02-19 | 2017-05-10 | 常州市第四制药厂有限公司 | Impurity of ulipristal acetate and preparation and detecting method of impurity |
| CN105566432B (en) * | 2016-02-19 | 2017-11-03 | 常州四药制药有限公司 | A kind of impurity of CDB-2914 and its preparation and detection method |
| CN106279326A (en) * | 2016-08-09 | 2017-01-04 | 南京臣功制药股份有限公司 | A kind of medroxyprogesterone acetate capsule have related substance and analyzing detecting method thereof |
-
2016
- 2016-08-09 CN CN201610647340.2A patent/CN106366149B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106366149A (en) | 2017-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Luo et al. | Simultaneous determination of thiamphenicol, florfenicol and florfenicol amine in swine muscle by liquid chromatography–tandem mass spectrometry with immunoaffinity chromatography clean-up | |
| CN102579612B (en) | Method for extracting total alkaloid of aconitum soongaricum | |
| CN102353732B (en) | Quality detection method of Zhenlong brain-refreshment preparation | |
| CN105017243B (en) | A kind of Ceftriaxone Sodium Photodegradation Products and preparation method thereof and analyzing detecting method | |
| CN102507825B (en) | Detecting method for effective components of traditional Chinese medicine Hugu capsules for preventing and treating osteoporosis | |
| CN106124645A (en) | Needle-based Solid-Phase Extraction filter | |
| CN101502549B (en) | Notoginsen triterpenes capsule as well as preparation method thereof and method for measuring content | |
| CN114280176A (en) | Method for detecting related substances in oxaagolide by using HPLC (high Performance liquid chromatography) | |
| CN106366149B (en) | The relevant material and its analyzing detecting method of a kind of medroxyprogesterone acetate dispersible tablet | |
| CN110927279B (en) | Method for separating imidapril hydrochloride related substances | |
| CN106279326A (en) | A kind of medroxyprogesterone acetate capsule have related substance and analyzing detecting method thereof | |
| CN107941946B (en) | Detection method of Vonoprazan fumarate | |
| CN103083388B (en) | Preparation method of fructus gleditsiae total saponins | |
| CN107167540B (en) | The method for measuring the DTPA-Zn in human urine biological sample | |
| CN114184716B (en) | High performance liquid chromatography analysis method for determining related substance components in halominosone cream | |
| CN106153795A (en) | Measure chenodeoxycholic acid crude drug content and the method having related substance thereof | |
| Levine | Column partition chromatography in pharmaceutical analysis | |
| CN108490095A (en) | A kind of method of Multiple components assay in pilose gerbera herb medicinal material | |
| CN103301081A (en) | Cefdinir dispersible tablet and preparation method thereof | |
| CN108445091B (en) | HPLC analysis method of estrone related substances | |
| CN106279191B (en) | Related substance in dextromethorphan hydrobromide guaiacol glycerol ether granule and its analyzing detecting method | |
| CN106290600A (en) | A kind of liquid chromatography separation health Buddhist nun replaces Buddhist nun and the method having related substance | |
| CN110988182B (en) | Quality detection method of Zhuang medicine ethnic medicine Huatuo Fengtongbao capsule | |
| CN111351866A (en) | Method for detecting hyodeoxycholic acid in Xihuang capsules | |
| CN104374855B (en) | The method of woodruff thuja acid and 10-deacetyl asperulosidic thuja acid content in HPLC Simultaneously test Noni juice |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |