CN112649531A - Method for detecting dexamethasone in reaction liquid in esterification stage in production process of dexamethasone sodium phosphate - Google Patents
Method for detecting dexamethasone in reaction liquid in esterification stage in production process of dexamethasone sodium phosphate Download PDFInfo
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- CN112649531A CN112649531A CN202011509433.1A CN202011509433A CN112649531A CN 112649531 A CN112649531 A CN 112649531A CN 202011509433 A CN202011509433 A CN 202011509433A CN 112649531 A CN112649531 A CN 112649531A
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- 229960003957 dexamethasone Drugs 0.000 title claims abstract description 53
- UREBDLICKHMUKA-CXSFZGCWSA-N dexamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-CXSFZGCWSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229960002344 dexamethasone sodium phosphate Drugs 0.000 title claims abstract description 25
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 23
- 239000012295 chemical reaction liquid Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 230000032050 esterification Effects 0.000 title claims abstract description 16
- PLCQGRYPOISRTQ-FCJDYXGNSA-L dexamethasone sodium phosphate Chemical compound [Na+].[Na+].C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)COP([O-])([O-])=O)(O)[C@@]1(C)C[C@@H]2O PLCQGRYPOISRTQ-FCJDYXGNSA-L 0.000 title 1
- VQODGRNSFPNSQE-CXSFZGCWSA-N dexamethasone phosphate Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)COP(O)(O)=O)(O)[C@@]1(C)C[C@@H]2O VQODGRNSFPNSQE-CXSFZGCWSA-N 0.000 claims abstract description 69
- 239000000243 solution Substances 0.000 claims abstract description 49
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229960004833 dexamethasone phosphate Drugs 0.000 claims abstract description 45
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000012490 blank solution Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000012085 test solution Substances 0.000 claims abstract description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000001514 detection method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 3
- VTLCNEGVSVJLDN-MLGOLLRUSA-N cefazedone Chemical compound S1C(C)=NN=C1SCC1=C(C(O)=O)N2C(=O)[C@@H](NC(=O)CN3C=C(Cl)C(=O)C(Cl)=C3)[C@H]2SC1 VTLCNEGVSVJLDN-MLGOLLRUSA-N 0.000 claims abstract description 3
- 229960005312 cefazedone Drugs 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 3
- 239000010452 phosphate Substances 0.000 claims abstract description 3
- 239000011550 stock solution Substances 0.000 claims description 16
- 239000000523 sample Substances 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000013558 reference substance Substances 0.000 claims description 8
- 230000014759 maintenance of location Effects 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 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
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The invention belongs to the technical field of detection methods, and particularly relates to a method for detecting dexamethasone in reaction liquid in an esterification stage in a production process of dexamethasone sodium phosphate, which comprises the following steps: (1) preparing a system applicability solution; (2) preparation of a test solution: taking 0.2ml of dexamethasone phosphate esterification reaction liquid, adding 0.1ml of concentrated hydrochloric acid and 1ml of water, shaking up, adding a mobile phase to dilute to 10ml, and mixing uniformly to obtain a test solution; (3) the blank solution is 10ml of mobile phase; (4) detecting the cefazedone phosphate in the test sample solution by adopting a high performance liquid chromatography; the preparation process of the mobile phase comprises the following steps: 45ml of triethylamine solution, 47.5ml of methanol and 7.5ml of acetonitrile are mixed uniformly to obtain a mobile phase. The method can detect whether the dexamethasone reacts completely in the esterification reaction of the dexamethasone sodium phosphate, control the content of dexamethasone serving as an impurity in the product and improve the yield.
Description
Technical Field
The invention belongs to the technical field of detection methods, and particularly relates to a method for detecting dexamethasone in reaction liquid in an esterification stage in a production process of dexamethasone sodium phosphate.
Background
In view of the above situation, we disclose a detection standard and a detection method for the dexamethasone phosphate reaction solution so as to better control the production process of dexamethasone sodium phosphate, thereby improving the product quality of the dexamethasone sodium phosphate.
Disclosure of Invention
The invention aims to provide a method for detecting dexamethasone in reaction liquid in an esterification stage in a production process of dexamethasone sodium phosphate. By detecting the dexamethasone phosphate in the reaction liquid in the esterification stage, the quality control condition of the dexamethasone sodium phosphate in the production process can be better mastered.
The realization process of the invention is as follows:
the method for detecting dexamethasone in reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate comprises the following steps:
(1) preparation of system suitability solution:
firstly, preparing a dexamethasone phosphate stock solution by using a dexamethasone phosphate reference substance and a methanol solvent;
then, preparing dexamethasone stock solution by using dexamethasone and a methanol solvent;
finally, precisely measuring 1ml of each of the dexamethasone phosphate solution and the dexamethasone solution, placing the dexamethasone phosphate solution and the dexamethasone solution into a 100ml volumetric flask, adding the mobile phase to scale, and shaking up to obtain a system applicability solution containing 10 mu g of dexamethasone phosphate and 10 mu g of dexamethasone per 1 ml;
(2) preparation of a test solution: taking 0.2ml of dexamethasone phosphate esterification reaction liquid, adding 0.1ml of concentrated hydrochloric acid and 1ml of water, shaking up, adding a mobile phase to dilute to 10ml, and mixing uniformly to obtain a test solution;
(3) the blank solution is 10ml of mobile phase;
(4) detecting the cefazedone phosphate in the test sample solution by adopting a high performance liquid chromatography;
the preparation process of the mobile phase comprises the following steps: 45ml of triethylamine solution, 47.5ml of methanol and 7.5ml of acetonitrile are mixed uniformly to obtain a mobile phase.
Further, in the step (1), the specific preparation process of the dexamethasone phosphate stock solution comprises the following steps: precisely weighing 25mg of dexamethasone phosphate reference substance, placing the dexamethasone phosphate reference substance in a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone phosphate stock solution;
the preparation process of the dexamethasone stock solution comprises the following steps: precisely weighing 25mg of dexamethasone, placing the dexamethasone into a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone stock solution.
Further, in the step (4), the chromatographic conditions of the high performance liquid chromatography are as follows:
a) flow rate: 1.0 ml/min;
b) detection wavelength: 242 nm;
c) column temperature: 30 ℃;
d) sample introduction amount: 20 mu l of the mixture;
e) packing and column length of chromatographic column: octadecylsilane chemically bonded silica, 250X 4.6 mm;
further, in the step (4), the preparation process of the triethylamine solution is as follows: 7.5ml of triethylamine is taken, water is added for dilution to 1000ml, and the pH value is adjusted to 3.0 +/-0.05 by phosphoric acid.
Further, in the step (4), the sample injection sequence of the high performance liquid chromatography is as follows: i) a blank solution; ii) a system suitability solution; iii) a test solution.
Further, in the step (4), the specific operation process of the high performance liquid chromatography is as follows: respectively taking 20 mu l of blank solution, 20 mu l of system applicability solution and 20 mu l of sample solution, sequentially injecting the blank solution, the system applicability solution and the sample solution into a high performance liquid chromatograph according to a sample injection sequence, recording a chromatogram until the retention time of a main component is 2 times, wherein in the system applicability solution chromatogram, the theoretical plate number is calculated according to a dexamethasone phosphate peak and is not less than 3000, and the separation degree of the dexamethasone phosphate and the dexamethasone phosphate peak is more than 4.4.
The invention has the advantages that: the method can detect whether the dexamethasone reacts completely in the esterification reaction of the dexamethasone sodium phosphate, control the content of dexamethasone serving as an impurity in the product and improve the yield.
Drawings
FIG. 1 is a chromatogram of a first run of a blank solution;
FIG. 2 is a graph of a peak table for a first run of a blank solution;
FIG. 3 is a chromatogram of a second run of a blank solution;
FIG. 4 is a graph of a peak table for a second run of a blank solution;
FIG. 5 is a chromatogram of a third run of a blank solution;
FIG. 6 is a peak chart of a third experiment of a blank solution;
FIG. 7 is a chromatogram of a first experiment of a system suitability solution;
FIG. 8 is a graph of a peak table for a first run of a system suitability solution;
FIG. 9 is a chromatogram of a second run of a system suitability solution;
FIG. 10 is a chart of peaks from a second run of a system suitability solution;
FIG. 11 is a chromatogram of a third run of a system suitability solution;
FIG. 12 is a chart of peaks from a third experiment of a system suitability solution;
FIG. 13 is a chromatogram of a first experiment of a test solution;
FIG. 14 is a graph of a peak profile for a first run of a test sample solution;
FIG. 15 is a chromatogram of a second experiment of a test solution;
FIG. 16 is a graph of a peak profile for a second experiment of a test sample solution;
FIG. 17 is a chromatogram of a third experiment of a test solution;
FIG. 18 is a graph of a peak profile for a third experiment of a test sample solution;
FIG. 19 is a schematic diagram of the reaction process for producing dexamethasone sodium phosphate from dexamethasone.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention discloses a method for detecting dexamethasone phosphate reaction solution by controlling the middle of an esterification stage in a production process of dexamethasone sodium phosphate so as to better monitor the middle process, thereby improving the product quality of the dexamethasone sodium phosphate.
Example 1
The method for detecting dexamethasone in reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate comprises the following steps:
(one) dexamethasone residues: HPLC
(II) instruments and appliances: analytical balance, pipette, high performance liquid chromatograph.
(III) reagent and test solution: dexamethasone, dexamethasone phosphate control, acetonitrile, methanol, triethylamine, phosphoric acid, concentrated hydrochloric acid (assay pure).
(IV) solution preparation
(1) Preparation of system suitability solution:
firstly, the specific preparation process of the dexamethasone phosphate stock solution comprises the following steps: precisely weighing 25mg of dexamethasone phosphate reference substance, placing the dexamethasone phosphate reference substance in a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone phosphate stock solution;
then, the specific preparation process of the dexamethasone stock solution is as follows: precisely weighing 25mg of dexamethasone, placing the dexamethasone into a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone stock solution;
finally, precisely measuring 1ml of each of the dexamethasone phosphate solution and the dexamethasone solution, placing the dexamethasone phosphate solution and the dexamethasone solution into a 100ml volumetric flask, adding the mobile phase to scale, and shaking up to obtain a system applicability solution containing 10 mu g of dexamethasone phosphate and 10 mu g of dexamethasone per 1 ml;
(2) preparation of a test solution: taking 0.2ml of dexamethasone phosphate esterification reaction liquid, adding 0.1ml of concentrated hydrochloric acid and 1ml of water, shaking up, adding a mobile phase to dilute to 10ml, and mixing uniformly to obtain a test solution;
(3) the blank solution is 10ml of mobile phase;
(V) chromatographic conditions and sequence arrangement
1. Flow rate: 1.0ml/min
2. Detection wavelength: 242nm
3. Column temperature: 30 deg.C
4. Sample introduction amount: 20 μ l
5. Packing and column length of chromatographic column: octadecylsilane chemically bonded silica, 250X 4.6mm
6. Mobile phase: 45ml of triethylamine solution, 47.5ml of methanol and 7.5ml of acetonitrile are uniformly mixed to obtain a mobile phase; the preparation process of the triethylamine solution comprises the following steps: 7.5ml of triethylamine is taken, water is added for dilution to 1000ml, and the pH value is adjusted to 3.0 +/-0.05 by phosphoric acid.
7. The sample injection sequence of the high performance liquid chromatography is as follows: i) a blank solution; ii) a system suitability solution; iii) a test solution.
8. The specific operation process of the high performance liquid chromatography is as follows: respectively taking 20 mu l of blank solution, 20 mu l of system applicability solution and 20 mu l of sample solution, sequentially injecting the blank solution, the system applicability solution and the sample solution into a high performance liquid chromatograph according to a sample injection sequence, recording a chromatogram until the retention time of a main component is 2 times, wherein in the system applicability solution chromatogram, the theoretical plate number is calculated according to a dexamethasone phosphate peak and is not less than 3000, and the separation degree of the dexamethasone phosphate and the dexamethasone phosphate peak is more than 4.4.
9. Sample injection sequence editing and result:
TABLE 1 sample introduction sequence editing and results
Note that: the blank solution is used in the sequence to eliminate test deviation caused by instrument and reagent contamination, and the sequence is the test sequence of a batch of samples, and three batches of measurement are carried out. If the measurement of multiple batches is carried out simultaneously, the blank sample injection times and the reference sample injection times are increased properly.
With reference to table 1 and fig. 1 to 18, it can be seen whether dexamethasone completely reacts or remains in the reaction solution during the esterification stage in the production process of dexamethasone sodium phosphate. As can be seen from FIGS. 7-12, the retention time of dexamethasone phosphate in the system suitability solution is about 15min, with an area% of 41, and the retention time of dexamethasone is about 19-20min, with an area% of 58. As can be seen from FIGS. 13-18, the retention time of dexamethasone phosphate was 15min at about 96 area%, the retention time of dexamethasone was about 19-20min at about 1 area%, indicating that the dexamethasone was substantially reacted completely with less residue.
Acceptance criteria: if a chromatographic peak corresponding to the dexamethasone peak-out time appears in the chromatogram of the test solution, the area percent is not more than 5.0 percent according to the area normalization method.
After the method is adopted, the dexamethasone phosphate in the middle process of the production of the dexamethasone sodium phosphate product is controlled, whether the dexamethasone reacts completely in the material dexamethasone in the esterification reaction of the dexamethasone sodium phosphate is controlled, the content of the impurity dexamethasone in the product is controlled, and the yield of the dexamethasone sodium phosphate product is improved.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and is not intended to limit the invention to the particular forms disclosed. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (6)
1. The method for detecting dexamethasone in reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate is characterized by comprising the following steps:
(1) preparation of system suitability solution:
firstly, preparing a dexamethasone phosphate stock solution by using a dexamethasone phosphate reference substance and a methanol solvent;
then, preparing dexamethasone stock solution by using dexamethasone and a methanol solvent;
finally, precisely measuring 1ml of each of the dexamethasone phosphate solution and the dexamethasone solution, placing the dexamethasone phosphate solution and the dexamethasone solution into a 100ml volumetric flask, adding the mobile phase to scale, and shaking up to obtain a system applicability solution containing 10 mu g of dexamethasone phosphate and 10 mu g of dexamethasone per 1 ml;
(2) preparation of a test solution: taking 0.2ml of dexamethasone phosphate esterification reaction liquid, adding 0.1ml of concentrated hydrochloric acid and 1ml of water, shaking up, adding a mobile phase to dilute to 10ml, and mixing uniformly to obtain a test solution;
(3) the blank solution is 10ml of mobile phase;
(4) detecting the cefazedone phosphate in the test sample solution by adopting a high performance liquid chromatography;
the preparation process of the mobile phase comprises the following steps: 45ml of triethylamine solution, 47.5ml of methanol and 7.5ml of acetonitrile are mixed uniformly to obtain a mobile phase.
2. The method for detecting dexamethasone in the reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the specific preparation process of the dexamethasone phosphate stock solution comprises the following steps: precisely weighing 25mg of dexamethasone phosphate reference substance, placing the dexamethasone phosphate reference substance in a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone phosphate stock solution;
the preparation process of the dexamethasone stock solution comprises the following steps: precisely weighing 25mg of dexamethasone, placing the dexamethasone into a 25ml volumetric flask, adding methanol for dissolving, fixing the volume to a scale, and shaking up to serve as dexamethasone stock solution.
3. The method for detecting dexamethasone in the reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the chromatographic conditions of the high performance liquid chromatography are as follows:
a) flow rate: 1.0 ml/min;
b) detection wavelength: 242 nm;
c) column temperature: 30 ℃;
d) sample introduction amount: 20 mu l of the mixture;
e) packing and column length of chromatographic column: octadecylsilane chemically bonded silica, 250X 4.6 mm;
4. the method for detecting dexamethasone in the reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the preparation process of the triethylamine solution is as follows: 7.5ml of triethylamine is taken, water is added for dilution to 1000ml, and the pH value is adjusted to 3.0 +/-0.05 by phosphoric acid.
5. The method for detecting dexamethasone in the reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the sample injection sequence of the high performance liquid chromatography is as follows: i) a blank solution; ii) a system suitability solution; iii) a test solution.
6. The method for detecting dexamethasone in the reaction liquid in the esterification stage in the production process of dexamethasone sodium phosphate as claimed in claim 5, wherein the method comprises the following steps: in the step (4), the specific operation process of the high performance liquid chromatography is as follows: respectively taking 20 mu l of blank solution, 20 mu l of system applicability solution and 20 mu l of sample solution, sequentially injecting the blank solution, the system applicability solution and the sample solution into a high performance liquid chromatograph according to a sample injection sequence, recording a chromatogram until the retention time of a main component is 2 times, wherein in the system applicability solution chromatogram, the theoretical plate number is calculated according to a dexamethasone phosphate peak and is not less than 3000, and the separation degree of the dexamethasone phosphate and the dexamethasone phosphate peak is more than 4.4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936809A (en) * | 2014-04-03 | 2014-07-23 | 上海新华联制药有限公司 | Improved preparation method of dexamethasone sodium phosphate intermediate |
| CN104490796A (en) * | 2014-12-19 | 2015-04-08 | 成都天台山制药有限公司 | Pharmaceutical composition of dexamethasone sodium phosphate for injection and preparation method of pharmaceutical composition |
| CN105136697A (en) * | 2015-08-18 | 2015-12-09 | 安徽城市药业有限责任公司 | Dexamethasone sodium phosphate injection intermediate testing method |
| US20170340644A1 (en) * | 2014-11-07 | 2017-11-30 | Santen Pharmaceutical Co., Ltd. | Ophthalmic aqueous composition |
-
2020
- 2020-12-18 CN CN202011509433.1A patent/CN112649531A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936809A (en) * | 2014-04-03 | 2014-07-23 | 上海新华联制药有限公司 | Improved preparation method of dexamethasone sodium phosphate intermediate |
| US20170340644A1 (en) * | 2014-11-07 | 2017-11-30 | Santen Pharmaceutical Co., Ltd. | Ophthalmic aqueous composition |
| CN104490796A (en) * | 2014-12-19 | 2015-04-08 | 成都天台山制药有限公司 | Pharmaceutical composition of dexamethasone sodium phosphate for injection and preparation method of pharmaceutical composition |
| CN105136697A (en) * | 2015-08-18 | 2015-12-09 | 安徽城市药业有限责任公司 | Dexamethasone sodium phosphate injection intermediate testing method |
Non-Patent Citations (3)
| Title |
|---|
| 李洁: "地塞米松磷酸钠注射液有关物质检查方法的探讨", 《中国药事》 * |
| 杨雪等: "高效液相色谱法测定地塞米松磷酸钠乳膏中地塞米松磷酸钠含量", 《中南药学》 * |
| 谭博: "地塞米松磷酸钠注射液有关物质检测方法探讨", 《科技与企业》 * |
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