CN103257190B - Method for measuring buprofen/famotidine compound preparation content - Google Patents
Method for measuring buprofen/famotidine compound preparation content Download PDFInfo
- Publication number
- CN103257190B CN103257190B CN201310129517.6A CN201310129517A CN103257190B CN 103257190 B CN103257190 B CN 103257190B CN 201310129517 A CN201310129517 A CN 201310129517A CN 103257190 B CN103257190 B CN 103257190B
- Authority
- CN
- China
- Prior art keywords
- famotidine
- mobile phase
- compound preparation
- brufen
- measuring
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring a buprofen/famotidine compound preparation content. The method comprises the following steps of: dissolving a compound preparation sample by methanol as a solvent; measuring by using a high performance liquid chromatography, wherein the measurement wavelength is 265nm; and with an octadecyl silane bonded silica gel filler as a stationary phase, performing gradient elution according to the following mobile phase conditions: the mobile phase A is a 0.02mol/L sodium acetate solution, pH is regulated to be 4.0 by using phosphoric acid, and the mobile phase B is acetonitrile. The method provided by the invention is time-saving and labor-saving, high in precision, accurate in content determination result and excellent in repeatability, and can be used for conventional analysis and quality control on the buprofen/famotidine compound preparation sample.
Description
Technical field
The present invention relates to a kind of method measuring brufen/famotidine compound preparation content, particularly a kind of method adopting high effective liquid chromatography for measuring brufen/famotidine compound preparation content, belongs to Pharmaceutical Analysis technical field.
Background technology
The chemical name of brufen is 2-(-4-isobutyl phenenyl) propionic acid, and molecular formula is C
13h
18o
2, molecular weight is 206.3.This medical instrument has anti-inflammatory, analgesia, refrigeration function, is applicable to treatment rheumatic arthritis, rheumatoid arthritis, osteoarthritis, ankylosing spondylitis and neuritis etc.
Famotidine chemical name is 3-[[[2-[(diamino methylene) is amino]-4-thiazolyl] methyl] sulfo-]-N-sulfonamide third amidine, and molecular formula is C
8h
15n
7o
2s
3, molecular weight is 337.5.This product is histamine H
2receptor antagonist.Have obvious inhibiting effect to gastric acid secretion, its action intensity is stronger than Cimetidine more than 30 times, stronger than ranitidine 6-10 times, clinical in gastric and duodenal ulcer, stress ulcer, acute gastric mucosal bleeding, gastrinoma and Reflux exophagitis etc.
Brufen has been proved possess both anti-inflammatory and pain relieving dual nature, and famotidine can reduce the gastric acid secretion that can cause gastric duodenal ulcer.Brufen and famotidine being made compound preparation, its alimentary canal security can be improved when not changing brufen pain relieving and anti-inflammatory performance.At present, FDA's approved composite tablet brufen/famotidine (800mg/26.6mg) goes on the market, for rheumatoid arthritis and the sings and symptoms of osteoarthritis, simultaneously reduction ulcer of upper digestive tract risk.
At present, prior art has disclosed the detection method using brufen or famotidine as the preparation of sole active agent, but still not for the detection method of content of brufen/famotidine compound preparation.Therefore, for better more promptly controlling the quality of brufen/famotidine compound preparation, find suitable chromatographic condition, thus obtain a kind of method adopting high effective liquid chromatography for measuring brufen/famotidine compound preparation content, this seems necessary.
Summary of the invention
In view of the deficiency of existing assay method, the object of the invention is to be studied by lot of experiments, a kind of method adopting high effective liquid chromatography for measuring brufen/famotidine compound preparation content is provided.This detection method can be used for the content detection of brufen/famotidine compound preparation sample, time saving and energy saving, is easy to operation.
In order to realize object of the present invention, inventor is studied by lot of experiments, finally obtains following technical scheme:
A kind of mensuration brufen/famotidine
1the method of compound preparation content, comprising described compound preparation sample with methyl alcohol is dissolution with solvents, high performance liquid chromatography is adopted to measure, determined wavelength is 265nm, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, gradient elution is carried out: mobile phase A is 0.02mol/L sodium acetate solution, with phosphorus acid for adjusting pH to 4.0 by following mobile phase condition; Mobile phase B is acetonitrile; The gradient of mobile phase arranges as follows:
| time (min) | mobile phase A | mobile phase B |
| 0 | 90 | 10 |
| 7 | 90 | 10 |
| 10 | 40 | 60 |
| 25 | 40 | 60 |
| 30 | 90 | 10 |
| 35 | 90 | 10. |
Preferably, the method for said determination brufen/famotidine compound preparation content, the overall flow rate of wherein said mobile phase is 1.0mL/min.
Further preferably, the method for said determination brufen/famotidine compound preparation content, the compound concentration after wherein said compound preparation sample is dissolved in methyl alcohol is brufen 3.0mg/mL, famotidine 0.1mg/mL.
Compared with prior art, the brufen that the present invention relates to/famotidine compound preparation content assaying method tool has the following advantages and significant progressive: time saving and energy saving, precision is high, assay result is accurate, reproducible, can be used for conventional analysis and the quality control of brufen/famotidine compound preparation sample.
Accompanying drawing explanation
Fig. 1 is the assay collection of illustrative plates of brufen/famotidine compound preparation sample.
Fig. 2 is the assay collection of illustrative plates of blank auxiliary sample.
Fig. 3 is the regression curve that the inventive method measures brufen standard items.
Fig. 4 is the regression curve that the inventive method measures famotidine standard items.
Embodiment
Form by the following examples, the brufen that the present invention relates to/famotidine compound preparation content assaying method is described in further detail, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following example, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1 high effective liquid chromatography for measuring brufen/famotidine compound preparation content
Getting brufen/famotidine compound preparation sample appropriate, take methyl alcohol as dissolution with solvents, adopts high performance liquid chromatography, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, by following mobile phase condition, detect by UV-detector, and calculate the content of brufen and famotidine by external standard method.
Mobile phase A: 3.28g anhydrous acetic acid sodium solution is dissolved in 1500mL water, with phosphorus acid for adjusting pH to 4.0, is then diluted with water to 2000mL.
Mobile phase B: acetonitrile.
Overall flow rate: 1.0mL/min
Wavelength: 265nm
Gradient
| Time (min) | Mobile phase A | Mobile phase B |
| 0 | 90 | 10 |
| 7 | 90 | 10 |
| 10 | 40 | 60 |
| 25 | 40 | 60 |
| 30 | 90 | 10 |
| 35 | 90 | 10 |
As shown in Figure 1, blank collection of illustrative plates as shown in Figure 2 for sample collection of illustrative plates.
From result, in chromatogram, famotidine went out peak at 7-5 minute, and brufen went out peak at 21-23 minute, and peak shape is good; On blank collection of illustrative plates, Interference Peaks does not all go out peak near above-mentioned two material main peaks.Viewed from integral result, suitable calculating, can calculate the content of famotidine and brufen according to external standard method
Computing formula is:
Wherein:
C
rrepresent the reference substance concentration of brufen/famotidine, unit is mg/mL;
A
rrepresent the reference substance peak area of brufen/famotidine;
A
srepresent the sample peak area of brufen/famotidine;
D represents extension rate;
W represents sample weighting amount, and unit is mg.
represent average loading amount, unit is mg.
C represents the labelled amount of brufen/famotidine, and unit is mg, and wherein brufen is 800mg, and famotidine is 26.6mg.
The precision development test of embodiment 2 assay method of the present invention
(1) linear
Getting brufen and famotidine reference substance appropriate, is dissolution with solvents with methyl alcohol in proportion, and press gradient concentration and dilute, adopt high performance liquid chromatography, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, by aforesaid flow phase condition sample introduction, detect with UV-detector 265nm wavelength place.With concentration (mg/mL) for horizontal ordinate, peak area is ordinate, draws regression curve, calculates regression coefficient.The results are shown in Table 1, Fig. 3, Fig. 4.
Table 1 typical curve
From result, brufen is good linear in 0.589 ~ 5.888mg concentration range; Famotidine is good linear within the scope of 0.0197 ~ 0.1970mg.
(2) repeatability
Get brufen/famotidine compound preparation sample appropriate, take methyl alcohol as dissolution with solvents, adopt high performance liquid chromatography, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, by aforesaid flow phase condition sample introduction, detect at 265nm wavelength place by UV-detector, and calculate the content of brufen and famotidine by external standard method.The results are shown in Table 2.
Table 2 is containing check weighing renaturation
From result, the repeatability of the content assaying method that the present invention relates to is good.
(2) recovery
Get brufen and famotidine, by recipe quantity preparation simulation prescription, measure content by preceding method.Calculate measured amount and the recovery, the results are shown in Table 3.
The table 3 titration recovery
From result, the recovery of content assaying method of the present invention is good, and wherein ibuprofen determination scope is between 640mg ~ 960mg, and famotidine measurement range is between 21.3 ~ 31.9mg.
From result, when sampling amount of the present invention is between 80% ~ 120% scope of ormal weight (brufen 800mg, famotidine 26.6mg), the recovery is good; This method is adopted to measure content accuracy high.
(3) sample determination
Get brufen/famotidine compound preparation sample appropriate, take methyl alcohol as dissolution with solvents, adopt high performance liquid chromatography, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, by following mobile phase condition, detect at 265nm wavelength place by UV-detector, and calculate the content of brufen and famotidine by external standard method.
Mobile phase A: anhydrous acetic acid sodium solution (3.28g---1500mL water), with phosphorus acid for adjusting pH to 4.0, is then diluted with water to 2000mL.
Mobile phase B: acetonitrile.
Overall flow rate: 1.0mL/min
Wavelength: 265nm
Gradient
| Time (min) | A | B |
| 0 | 90 | 10 |
| 7 | 90 | 10 |
| 10 | 40 | 60 |
| 25 | 40 | 60 |
| 30 | 90 | 10 |
| 35 | 90 | 10 |
The results are shown in Table 4.
Table 4 sample size measures
Through methodological study, content assaying method of the present invention, has good specificity, accuracy, precision, is suitable for the assay of brufen and famotidine.
Table 5 content assaying method checking of the present invention is summed up
Claims (1)
1. one kind measures the method for brufen/famotidine compound preparation content, it is characterized in that: comprising described compound preparation sample with methyl alcohol is dissolution with solvents, high performance liquid chromatography is adopted to measure, determined wavelength is 265nm, with octadecylsilane chemically bonded silica filling agent for Stationary liquid, gradient elution is carried out: mobile phase A is 0.02mol/L sodium acetate solution, with phosphorus acid for adjusting pH to 4.0 by following mobile phase condition; Mobile phase B is acetonitrile; The gradient of mobile phase arranges as follows:
, the overall flow rate of mobile phase is 1.0mL/min, and the compound concentration after described compound preparation sample is dissolved in methyl alcohol is brufen 3.0mg/mL, famotidine 0.1mg/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310129517.6A CN103257190B (en) | 2013-04-15 | 2013-04-15 | Method for measuring buprofen/famotidine compound preparation content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310129517.6A CN103257190B (en) | 2013-04-15 | 2013-04-15 | Method for measuring buprofen/famotidine compound preparation content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103257190A CN103257190A (en) | 2013-08-21 |
| CN103257190B true CN103257190B (en) | 2015-02-25 |
Family
ID=48961230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310129517.6A Active CN103257190B (en) | 2013-04-15 | 2013-04-15 | Method for measuring buprofen/famotidine compound preparation content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103257190B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568853A (en) * | 2016-12-30 | 2017-04-19 | 山东康美乐医药科技有限公司 | A method of detecting impurities in a lapatinib intermediate |
| CN109613128A (en) * | 2018-11-14 | 2019-04-12 | 上海信谊万象药业股份有限公司 | The measuring method of drug content in a kind of Famotidine Capsule |
| CN110286182A (en) * | 2019-07-31 | 2019-09-27 | 太原市食品药品检验所 | The method for detecting ranitidine hydrochloride, Cimetidine, famotidine, nizatidine, Lafutidine |
| CN110579542B (en) * | 2019-09-04 | 2022-04-05 | 北京悦康科创医药科技股份有限公司 | Method for measuring ranitidine hydrochloride related substances by high performance liquid chromatography |
| CN112526013B (en) * | 2020-11-20 | 2022-09-06 | 人福普克药业（武汉）有限公司 | Method for detecting concentration of related substances in ibuprofen medicament by using ultra-high liquid chromatography |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011050259A1 (en) * | 2009-10-22 | 2011-04-28 | Eiger Health Partners, Llc | Compositions, methods for treatment, and diagnoses of autoimmunity-related disorders and methods for making such compositions |
| CN102854263A (en) * | 2012-08-31 | 2013-01-02 | 石家庄中硕药业集团有限公司 | Method for simultaneous determination of content of ibuprofen and arginine in ibuprofen injection |
-
2013
- 2013-04-15 CN CN201310129517.6A patent/CN103257190B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011050259A1 (en) * | 2009-10-22 | 2011-04-28 | Eiger Health Partners, Llc | Compositions, methods for treatment, and diagnoses of autoimmunity-related disorders and methods for making such compositions |
| CN102854263A (en) * | 2012-08-31 | 2013-01-02 | 石家庄中硕药业集团有限公司 | Method for simultaneous determination of content of ibuprofen and arginine in ibuprofen injection |
Non-Patent Citations (3)
| Title |
|---|
| Development and Validation of Liquid ChromatographicMethod for Estimation of Ibuprofen and Famotidine in Combined Dosage Form;Dimal A. Shah等;《ISRN Analytical Chemistry》;20121231;第2012卷;第1-5页 * |
| RP-UPLC method development and validation for the simultaneous estimation of ibuprofen and famotidine in pharmaceutical dosage form;Yarram Ramakoti Reddy等;《Pharmaceutical Methods》;20121231;第3卷(第2期);第58页Chromatographic conditions和Preparation of sample solution节 * |
| V. Rajani Sekhar等.RP-HPLC and UV-derivative spectrophotometry technique for the simultaneous estimation of ibuprofen and famotidine in pharmaceutical dosage form.《Der Pharmacia Sinica》.2013,第4卷(第2期),第160-170页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103257190A (en) | 2013-08-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103257190B (en) | Method for measuring buprofen/famotidine compound preparation content | |
| CN103175905B (en) | Method for determining impurities in febuxostat and its preparation through high performance liquid chromatography | |
| CN105334274B (en) | Reversed-phase high performance liquid chromatography determination method for content and related substances of tofacitinib citrate | |
| CN103713077B (en) | The method of alpha-aminobutyric acid content in high effective liquid chromatography for measuring red colouring agent for food, also used as a Chinese medicine | |
| WO2011012848A8 (en) | Improvements relating to sensor devices | |
| CN104458965B (en) | Content of iodine detection method in a kind of feed | |
| CN104251889A (en) | Method for determining content of three components comprising phenylephrine hydrochloride, chlorphenamine maleate and ibuprofen in compound cold treatment tablet | |
| CN103698430B (en) | Esomeprazole sodium and method for detecting impurity content in esomeprazole sodium for injection | |
| CN107727773B (en) | Method for detecting purity of oxitinib mesylate by adopting liquid chromatography | |
| CN106525994B (en) | Method for determining related substances of paracetamol and tramadol capsule | |
| Trivedi et al. | A rapid, stability indicating RP-UPLC method for determination of paliperidone palmitate in a depot injectable formulation | |
| CN103099795A (en) | Indometacin sustained release tablet, preparation method thereof, as well as release controlling method and standard | |
| CN101191787B (en) | High performance liquid chromatography method for measuring doripenem content | |
| CN102269749A (en) | Method for detecting adenosine content in hericium erinaceus tablet | |
| CN111307990B (en) | Method for simultaneously determining content of cystine and methionine in artificial tiger bone powder | |
| CN103743711A (en) | Method for detecting gibberellins in food by using cyclodextrin and fluorescence resonance energy transfer technology | |
| CN108072717A (en) | A kind of detection method of arginine solution | |
| Bajerski et al. | Determination of cetirizine in tablets and compounded capsules: comparative study between CE and HPLC | |
| CN102012406A (en) | Quality detection method of thiamphenicol glycinate hydrochloride | |
| CN110441437A (en) | A kind of measuring method of Michaelis acid content | |
| CN111157638A (en) | Method for detecting oxalic acid content in vitamin C | |
| CN104569260A (en) | Method for detecting residual amount of formaldehyde in colistimethate sodium | |
| Pradhan et al. | Development and validation of a stability indicating RP-HPLC method for the determination of valsartan | |
| CN108107120B (en) | Method for measuring intermediate product 6, 6-dibromo penicillanic acid by adopting high performance liquid chromatography | |
| Farouk et al. | Novel validated chromatographic method for determination of some anti-hypertensive drugs |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |