CN104931632A - Method for detecting residual tartaric acid amount in moxifloxacin hydrochloride - Google Patents
Method for detecting residual tartaric acid amount in moxifloxacin hydrochloride Download PDFInfo
- Publication number
- CN104931632A CN104931632A CN201410105498.8A CN201410105498A CN104931632A CN 104931632 A CN104931632 A CN 104931632A CN 201410105498 A CN201410105498 A CN 201410105498A CN 104931632 A CN104931632 A CN 104931632A
- Authority
- CN
- China
- Prior art keywords
- solution
- moxifloxacin hydrochloride
- detection method
- mobile phase
- diethylamine
- 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.)
- Granted
Links
- 229960005112 moxifloxacin hydrochloride Drugs 0.000 title claims abstract description 44
- IDIIJJHBXUESQI-DFIJPDEKSA-N moxifloxacin hydrochloride Chemical compound Cl.COC1=C(N2C[C@H]3NCCC[C@H]3C2)C(F)=CC(C(C(C(O)=O)=C2)=O)=C1N2C1CC1 IDIIJJHBXUESQI-DFIJPDEKSA-N 0.000 title claims abstract description 40
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title abstract description 13
- 235000002906 tartaric acid Nutrition 0.000 title abstract 4
- 239000011975 tartaric acid Substances 0.000 title abstract 4
- 239000000243 solution Substances 0.000 claims abstract description 48
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 28
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 19
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 26
- 229940095064 tartrate Drugs 0.000 claims description 26
- 239000012071 phase Substances 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 13
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 claims description 12
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 239000013558 reference substance Substances 0.000 claims description 6
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 229960003702 moxifloxacin Drugs 0.000 claims description 3
- FABPRXSRWADJSP-MEDUHNTESA-N moxifloxacin Chemical compound COC1=C(N2C[C@H]3NCCC[C@H]3C2)C(F)=CC(C(C(C(O)=O)=C2)=O)=C1N2C1CC1 FABPRXSRWADJSP-MEDUHNTESA-N 0.000 claims description 3
- 238000010568 chiral column chromatography Methods 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000004296 chiral HPLC Methods 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 12
- 238000000926 separation method Methods 0.000 description 5
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 150000007660 quinolones Chemical class 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- 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 detecting the residual tartaric acid amount in moxifloxacin hydrochloride. The high performance liquid chromatography (HPLC) is adopted to detect the tartaric acid; an AD-H chiral HPLC column is adopted, the fluid phase is composed of an n-hexane solution containing trifluoroacetic acid and an ethanol solution containing diethylamine, and the detection wavelength is 205 nm. The provided method has the advantages of good linearity, high sample injection precision, stable solution within 12hours, and accurate and reliable recovery rate, is capable of precisely measuring the residual amount of tartaric acid in moxifloxacin hydrochloride, and is benefit for the comprehensive research on moxifloxacin hydrochloride.
Description
Technical field
The present invention relates to drug quality detection method, particularly the detection method of moxifloxacin hydrochloride mesotartaric acid residual quantity.
Background technology
Moxifloxacin hydrochloride is forth generation quinolones broad spectrum antibiotic, is used for the treatment of the infection such as respiratory tract and skin.
Tartrate may be had in moxifloxacin hydrochloride building-up process remain, because tartrate only has end to absorb, absorption is had at 205nm place, at the 293nm place of moxifloxacin hydrochloride maximum absorption wavelength without absorbing, and due to tartrate polarity comparatively large, under moxifloxacin hydrochloride related substance detects chromatographic condition, tartrate is almost without reserve, therefore need to set up moxifloxacin hydrochloride mesotartaric acid residues detection method, to ensure drug quality.
Summary of the invention
The object of the present invention is to provide a kind of detection method of moxifloxacin hydrochloride mesotartaric acid residual quantity, go out the residual quantity of moxifloxacin hydrochloride mesotartaric acid with Accurate Determining, ensure drug quality.
Moxifloxacin hydrochloride mesotartaric acid residual quantity inspection side of the present invention method, detected by high performance liquid chromatography, chromatographic column adopts AD-H chiral chromatographic column, and mobile phase is the mixed liquor of the hexane solution containing trifluoroacetic acid and the ethanolic solution containing diethylamine, and determined wavelength is 205nm.
Further, the preferred wherein trifluoroacetic acid content of the above-mentioned hexane solution containing trifluoroacetic acid is 0.1 ~ 0.5%(percent by volume), most preferably be 0.3%.
The preferred wherein diethylamine content of the above-mentioned ethanolic solution containing diethylamine is 0.1 ~ 0.4%(percent by volume), most preferably be 0.2%.
In above-mentioned mobile phase, the volume ratio of the hexane solution containing trifluoroacetic acid and the ethanolic solution containing diethylamine is preferably 75 ~ 85:15 ~ 25, most preferably is 80:20.
The specification of above-mentioned AD-H chiral chromatographic column is 250mm × 4.6mm, 5 μm; During detection, the flow velocity of mobile phase is 0.3 ~ 1.0ml/min, is preferably 0.5ml/min.
In one particular embodiment of the present invention, described high-efficient liquid phase chromatogram condition is: chromatographic column AD-H post, chromatographic column specification: 250mm × 4.6mm, 5 μm; Normal hexane-containing the ethanol=80:20(volume ratio of 0.2% diethylamine with containing 0.3% trifluoroacetic acid) for mobile phase, determined wavelength 205nm, flow velocity 0.5ml/min.
Concrete determination method can be: get moxifloxacin hydrochloride product to be tested appropriate, adds proper amount of methanol and dissolve after accurately weighed, makes the hydrochloric MOXIFLOXACIN 2mg ~ 3mg(of every 1ml as 3mg with mobile phase dilution) solution, shake up, as need testing solution; Separately get tartrate reference substance appropriate, accurately weighed rear proper amount of methanol is dissolved, and makes every 1ml containing tartrate 0.15mg ~ 0.30mg(as 0.15mg with mobile phase dilution) solution, shake up, in contrast product solution; Precision measures need testing solution and each 10 μ l of reference substance solution, respectively injection liquid chromatography, record chromatogram; If any tartaric chromatographic peak in the chromatogram of need testing solution, by external standard method, with calculated by peak area, draw moxifloxacin hydrochloride product to be tested mesotartaric acid residual quantity.
Moxifloxacin hydrochloride mesotartaric acid residues detection method provided by the invention, have linear good, sample introduction precision good, solution is stable in 12 hours, the recovery result advantage such as accurately and reliably, the method can go out the residual quantity of moxifloxacin hydrochloride mesotartaric acid, for comprehensive research of moxifloxacin hydrochloride related substance provides effective method by Accurate Determining.
Accompanying drawing explanation
Fig. 1 is the chromatogram of solvent methanol and mobile phase (MP);
Fig. 2 is tartaric chromatogram;
Fig. 3 is moxifloxacin hydrochloride chromatogram;
Fig. 4 is that the HPLC of tartrate and moxifloxacin hydrochloride system suitability schemes.
Embodiment
Below by instantiation, the present invention is described further, but the scope do not limited the present invention in any way.
Chromatographic condition
To apply the chiral chromatographic column (AD-H post 250mm × 4.6mm, 5 μm) that amylose-three-(3,5-xylyl carbamate) silica gel is Stationary liquid; With normal hexane (containing 0.3% trifluoroacetic acid)-ethanol (containing 0.2% diethylamine)=80:20(volume ratio) be mobile phase (MP), determined wavelength 205nm, flow velocity 0.5ml/min.
Determination method
Get moxifloxacin hydrochloride product to be tested appropriate, accurately weighed, add proper amount of methanol and dissolve, make the solution of the hydrochloric MOXIFLOXACIN 3mg of every 1ml with mobile phase dilution, shake up, as need testing solution; Separately get tartrate reference substance appropriate, accurately weighed, dissolve by proper amount of methanol, the solution of every 1ml containing tartrate 0.15mg is made in mobile phase dilution, shakes up, in contrast product solution.Precision measures need testing solution and each 10 μ l of reference substance solution, respectively injection liquid chromatography, record chromatogram.If any tartaric chromatographic peak in the chromatogram of need testing solution, by external standard method, with calculated by peak area.
Each sample solution is located
1), get solvent methanol, mobile phase direct injected mensuration, chromatogram is shown in Fig. 1;
2), tartrate: get tartrate 20.23mg, put in 10ml measuring bottle, dissolve by proper amount of methanol, mobile phase is diluted to scale, and chromatogram is shown in Fig. 2;
3), moxifloxacin hydrochloride: get moxifloxacin hydrochloride 10.5g, accurately weighed, put in 10ml measuring bottle, dissolve by proper amount of methanol, mobile phase is diluted to scale, and chromatogram is shown in Fig. 3;
4), tartrate and moxifloxacin hydrochloride mixed solution: chromatogram is shown in Fig. 4.
As can be seen from Fig. 1 to Fig. 4, tartrate and moxifloxacin hydrochloride can baseline separation, and solvent methanol and mobile phase do not disturb the detection of moxifloxacin hydrochloride mesotartaric acid.
System suitability
Get tartrate and be about 11mg, moxifloxacin hydrochloride is about 75mg, accurately weighed, puts in same 25ml measuring bottle, and add proper amount of methanol and dissolve, mobile phase is diluted to scale, shakes up, as system suitability solution.Get system suitability solution 10 μ l, injection liquid chromatography, record chromatogram, see accompanying drawing 4, the degree of separation of tartrate and moxifloxacin hydrochloride should be greater than 1.0.Continuous sample introduction 6 pin, records RSD% and the degree of separation of the peak area of two chromatographic peaks, sees the following form.
Moxifloxacin hydrochloride mesotartaric acid detection system applicability result
| Sample | Tartrate retention time | Moxifloxacin hydrochloride retention time | Tartrate peak area | Degree of separation |
| 1 | 15.943 | 19.056 | 737687 | 2.80 |
| 2 | 15.976 | 19.003 | 735296 | 2.72 |
| 3 | 15.986 | 18.965 | 743716 | 2.66 |
| 4 | 15.98 | 18.95 | 734083 | 2.65 |
| 5 | 15.998 | 18.931 | 737567 | 2.62 |
| 6 | 16.009 | 18.904 | 740236 | 2.57 |
| On average | 15.98 | 18.97 | 738097.50 | 2.67 |
| S | 0.02 | 0.05 | 3480.09 | 0.08 |
| RSD% | 0.14 | 0.29 | 0.47 | 2.95 |
Conclusion: as can be seen from the above results, the degree of separation 2.65 of tartrate and moxifloxacin hydrochloride, the RSD% of tartrate peak area is 0.47%.Illustrative system applicability meets test request.
The range of linearity:
Tartrate is good in 91.20 μ g/ml ~ 304.20 μ g/ml scope internal linear; Moxifloxacin hydrochloride is good in 31.50 μ g/ml ~ 105.00 μ g/ml scope internal linear.
Minimum detectability:
Record tartaric minimum being quantitatively limited to and be less than 1000ng.
Sample introduction precision:
Continuous sample introduction 6 times, the RSD% of moxifloxacin hydrochloride retention time and peak area is less than 2%, and sample introduction precision is good.
Stability of solution:
Get the need testing solution in sample introduction precision test, room temperature is placed, and measures respectively at different time sample introduction, investigates stability of solution.Conclusion: moxifloxacin hydrochloride sample solution room temperature is placed, and in 12 hours, the RSD% of peak area is 2.70%, basicly stable in solution 12 hours.
Recovery test:
The RSD of the recovery of high, medium and low 3 concentration 9 increment product, all in 98.0 ~ 102.0% scopes, meets mensuration requirement.
The determination of residual amount of moxifloxacin hydrochloride three batch sample tartrate
According to the aforementioned moxifloxacin hydrochloride mesotartaric acid residual quantity inspection method determined, check three batch samples, result is as follows.
Moxifloxacin hydrochloride three batch sample tartrate determination of residual amount result
| Lot number | 20110301 | 20110302 | 20110303 |
| Tartrate % | Do not detect | Do not detect | Do not detect |
Conclusion: three batch sample tartrate residual quantity inspections are all less than 1.0%.
Conclusion: by above-mentioned moxifloxacin hydrochloride mesotartaric acid residue checking, method is linear well, sample introduction precision is good, solution is stable in 12 hours, recovery result accurately and reliably, therefore known set up method can go out the residual quantity of moxifloxacin hydrochloride mesotartaric acid, for comprehensive research of moxifloxacin hydrochloride related substance provides effective method by Accurate Determining.
Claims (9)
1. the detection method of a moxifloxacin hydrochloride mesotartaric acid residual quantity, detected by high performance liquid chromatography, chromatographic column adopts AD-H chiral chromatographic column, and mobile phase is the mixed liquor of the hexane solution containing trifluoroacetic acid and the ethanolic solution containing diethylamine, and determined wavelength is 205nm.
2. detection method as claimed in claim 1, is characterized in that, described is 0.1 ~ 0.5% containing trifluoroacetic acid content in the hexane solution of trifluoroacetic acid.
3. detection method as claimed in claim 1, is characterized in that, described is 0.1 ~ 0.4% containing diethylamine content in the ethanolic solution of diethylamine.
4. detection method as claimed in claim 1, is characterized in that, the volume ratio of the described hexane solution containing trifluoroacetic acid and the ethanolic solution containing diethylamine is 75 ~ 85:15 ~ 25.
5. detection method as claimed in claim 1, it is characterized in that, the specification of described AD-H chiral chromatographic column is 250mm × 4.6mm, 5 μm.
6. detection method as claimed in claim 1, it is characterized in that, the flow velocity of mobile phase is 0.3 ~ 1.0ml/min.
7. detection method as claimed in claim 1, it is characterized in that, high-efficient liquid phase chromatogram condition is: adopt AD-H chiral column chromatography post, chromatographic column specification: 250mm × 4.6mm, 5 μm; With containing the hexane solution of 0.2 ~ 0.5% trifluoroacetic acid: containing the mixed liquor of ethanolic solution=75 ~ 85:15 ~ 25 volume ratio of 0.1 ~ 0.4% diethylamine for mobile phase; Determined wavelength 205nm; Flow velocity 0.3 ~ 1.0ml/min.
8. detection method as claimed in claim 7, it is characterized in that, high-efficient liquid phase chromatogram condition is: adopt AD-H chiral chromatographic column, chromatographic column specification: 250mm × 4.6mm, 5 μm; With containing the hexane solution of 0.3% trifluoroacetic acid: containing the mixed liquor of the ethanolic solution=80:20 volume ratio of 0.2% diethylamine for mobile phase; Determined wavelength 205nm; Flow velocity 0.5ml/min.
9. the detection method as described in as arbitrary in claim 1 ~ 8, it is characterized in that, concrete detecting step comprises:
1) get moxifloxacin hydrochloride product to be tested appropriate, add proper amount of methanol after accurately weighed and dissolve, make the solution of the hydrochloric MOXIFLOXACIN 2mg ~ 3mg of every 1ml with mobile phase dilution, shake up, as need testing solution;
2) get tartrate reference substance appropriate, accurately weighed rear proper amount of methanol is dissolved, and makes the solution of every 1ml containing tartrate 0.15 ~ 0.30mg, shake up, in contrast product solution with mobile phase dilution;
3) precision measures need testing solution and each 10 μ l of reference substance solution, respectively injection liquid chromatography, record chromatogram;
4) if any tartaric chromatographic peak in the chromatogram of need testing solution, by external standard method, with calculated by peak area, moxifloxacin hydrochloride product to be tested mesotartaric acid residual quantity is drawn.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105498.8A CN104931632B (en) | 2014-03-20 | 2014-03-20 | Moxifloxacin hydrochloride mesotartaric acid residues detection method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105498.8A CN104931632B (en) | 2014-03-20 | 2014-03-20 | Moxifloxacin hydrochloride mesotartaric acid residues detection method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104931632A true CN104931632A (en) | 2015-09-23 |
| CN104931632B CN104931632B (en) | 2017-08-25 |
Family
ID=54118899
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410105498.8A Expired - Fee Related CN104931632B (en) | 2014-03-20 | 2014-03-20 | Moxifloxacin hydrochloride mesotartaric acid residues detection method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104931632B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111089906A (en) * | 2018-10-23 | 2020-05-01 | 江苏正大丰海制药有限公司 | Separation method of moxifloxacin hydrochloride and moxifloxacin tartrate |
| CN112986468A (en) * | 2019-12-13 | 2021-06-18 | 武汉九州钰民医药科技有限公司 | Analysis method for detecting ciprofloxacin chloride in ciprofloxacin hydrochloride tablet |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05139999A (en) * | 1991-11-25 | 1993-06-08 | Sumika Bunseki Center:Kk | Chirality-identifying agent and separator for chromatography |
| CN101101284A (en) * | 2007-07-26 | 2008-01-09 | 复旦大学 | Method for simultaneously determining multiple organic acid content of fruit |
| CN101531602A (en) * | 2008-03-10 | 2009-09-16 | 北京德众万全医药科技有限公司 | Method for analyzing and separating formoterol tartrate intermediate by using HPLC method |
| CN102818872A (en) * | 2012-08-08 | 2012-12-12 | 福建省农业科学院农业工程技术研究所 | High performance liquid chromatography for simultaneously detecting content of ten organic acids in fruit |
-
2014
- 2014-03-20 CN CN201410105498.8A patent/CN104931632B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05139999A (en) * | 1991-11-25 | 1993-06-08 | Sumika Bunseki Center:Kk | Chirality-identifying agent and separator for chromatography |
| CN101101284A (en) * | 2007-07-26 | 2008-01-09 | 复旦大学 | Method for simultaneously determining multiple organic acid content of fruit |
| CN101531602A (en) * | 2008-03-10 | 2009-09-16 | 北京德众万全医药科技有限公司 | Method for analyzing and separating formoterol tartrate intermediate by using HPLC method |
| CN102818872A (en) * | 2012-08-08 | 2012-12-12 | 福建省农业科学院农业工程技术研究所 | High performance liquid chromatography for simultaneously detecting content of ten organic acids in fruit |
Non-Patent Citations (4)
| Title |
|---|
| HAIFENGPAN 等: "Immobilizationof Escherichiacoli cells with cis-epoxysuccinate hydrolase activityfor D(-)-tartaric acid production", 《BIOTECHNOL LETT》 * |
| MIRIAM SCHNITZLER 等: "Trans-Aconitic acid, glucosylflavones and hydroxycinnamoyltartaric acids from the leaves of Echinodorus grandiflorus ssp. aureus, a Brazilian medicinal plant", 《REVISTA BRASILEIRA DE FARMACOGNOSIA》 * |
| 刘颖 等: "酒石酸和氰基二苯基二氢吡唑的高效液相色谱手性分离", 《分析科学学报》 * |
| 李金昶 等: "高效液相色谱法分离和测定酒石酸和马来酸", 《分子科学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111089906A (en) * | 2018-10-23 | 2020-05-01 | 江苏正大丰海制药有限公司 | Separation method of moxifloxacin hydrochloride and moxifloxacin tartrate |
| CN112986468A (en) * | 2019-12-13 | 2021-06-18 | 武汉九州钰民医药科技有限公司 | Analysis method for detecting ciprofloxacin chloride in ciprofloxacin hydrochloride tablet |
| CN112986468B (en) * | 2019-12-13 | 2024-05-03 | 武汉九州钰民医药科技有限公司 | Analysis method for detecting ciprofloxacin chloride in ciprofloxacin hydrochloride tablet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104931632B (en) | 2017-08-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104655751B (en) | A kind of detect the method for organic solvent residual in dapoxetine | |
| CN111855881B (en) | Method for detecting hydroxylamine hydrochloride in azilsartan | |
| CN104062375A (en) | Method for detecting drug and enantiomer impurities of drug | |
| CN106596798B (en) | Analysis method of related substances in vortioxetine hydrobromide | |
| CN103592379A (en) | Analytic method of omeprazole related substance | |
| CN105203658A (en) | Detection method for residual solvent in ezetimibe | |
| CN103063769B (en) | Quality detecting method for mecobalamine capsule | |
| CN102375033A (en) | High performance liquid chromatographic analysis method of bendamustine hydrochloride and its related substances | |
| CN102841170A (en) | Method for detecting impurity phenylhydrazine in edaravone | |
| CN104931632A (en) | Method for detecting residual tartaric acid amount in moxifloxacin hydrochloride | |
| CN104730165A (en) | High performance liquid chromatography (HPLC) detection method of Rivaroxaban | |
| CN103604887A (en) | Method for measuring residual solvent of cephalosporin medicines | |
| CN103760260A (en) | Method for determining related substances of bilastine intermediate by using high-performance liquid chromatography | |
| CN105866268B (en) | Detection method that is a kind of while determining a variety of bacteriostatic agents in eye drops | |
| CN104833740A (en) | HPLC (High Performance Liquid Chromatography) method for rivaroxaban intermediate | |
| CN108398497B (en) | High performance liquid chromatography detection method of tris (nonylphenol) phosphite ester | |
| CN103163228A (en) | Efficient liquid phase analysis method for hydroxyfasudil and preparation thereof | |
| CN102901784A (en) | Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals | |
| CN106198819A (en) | The method of residual solvent in Headspace Gas Chromatography sitagliptin crude drug | |
| CN106525994A (en) | Method for determination of related substances of paracetamol and tramadol hydrochloride capsules | |
| CN103543231B (en) | The method for separating and analyzing of chloroform residual quantity in a kind of meclozine hydrochloride | |
| CN105606746A (en) | HPLC (high-performance liquid chromatography) detection method for octylated diphenylamine in lansoprazole | |
| CN104535690A (en) | Method for measuring content of cinnarizine in cinnarizine solid preparation | |
| CN102636597A (en) | Method for measuring residual solvent in tetracycline hydrochloride bulk drug by utilizing headspace gas chromatography | |
| CN105628807B (en) | A kind of quality determining method of the amino piperidines of 1 Boc 4 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221014 Address after: 3007, Hengqin international financial center building, No. 58, Huajin street, Hengqin new area, Zhuhai, Guangdong 519031 Patentee after: New founder holdings development Co.,Ltd. Patentee after: PKUCARE PHARMACEUTICAL R&D CENTER Patentee after: Peking University Medical Management Co.,Ltd. Address before: 100871, fangzheng building, 298 Fu Cheng Road, Beijing, Haidian District Patentee before: PEKING UNIVERSITY FOUNDER GROUP Co.,Ltd. Patentee before: PKUCARE PHARMACEUTICAL R&D CENTER Patentee before: PKU HEALTHCARE INDUSTRY Group |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170825 |