CN111380969A - Detection method for content of fluticasone furoate and related substances - Google Patents
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- XTULMSXFIHGYFS-VLSRWLAYSA-Nfluticasone furoateChemical compoundO([C@]1([C@@]2(C)C[C@H](O)[C@]3(F)[C@@]4(C)C=CC(=O)C=C4[C@@H](F)C[C@H]3[C@@H]2C[C@H]1C)C(=O)SCF)C(=O)C1=CC=CO1XTULMSXFIHGYFS-VLSRWLAYSA-N0.000titleclaimsabstractdescription37
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- 239000000377silicon dioxideSubstances0.000claimsabstractdescription15
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- 229940079593drugDrugs0.000abstractdescription8
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- 238000006731degradation reactionMethods0.000abstractdescription3
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- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
Description
Technical Field
The invention belongs to the field of pharmaceutical analysis, and particularly relates to a method for detecting the content of fluticasone furoate and related substances.
Background
Fluticasone furoate (Fluticasone furoate) is an artificially synthesized corticosteroid derived from Fluticasone, belongs to glucocorticoid, shows high affinity with human glucocorticoid receptor in vitro, and has strong anti-inflammatory effect. Treating respiratory system diseases such as allergic rhinitis, asthma, COPD, etc.
Since the research on impurities of compounds is related to the safety of medicines, and the research and detection requirements on impurities in bulk drugs are higher and higher with the increase of the evaluation of medicines in recent years, the development of analysis methods thereof is particularly important. At present, both domestic and foreign documents and pharmacopoeias do not disclose a related substance analysis method of a furoic acid fluticasone raw material medicament and a preparation thereof. For bulk drugs, the impurities generally include process impurities and degradation impurities; different synthetic routes and processes produce different impurities, and the company separates and prepares the impurities of the furoic acid fluticasone, including: FFZ6, FFZ14, FFZ17, FZ11, FFZ1, FFZ16, FFZ3, FFZ5, FFZ12, FFZ15 and FFZ2, wherein the structural formulas of FFZ16, FFZ17, FFZ3 and FFZ15 are shown in the specification, and the structures of other impurities are confirmed.
The Asian Journal of Pharmaceutical and Clinical Research (2017),10(4),302-305 uses UV spectrophotometry to simultaneously determine the content of fluticasone furoate and vilanterol, but the method is UV spectrophotometry and cannot be used for detecting related substances of fluticasone furoate. Therefore, in order to better control the impurities of the medicine and further ensure the safety of the medicine, a set of related substance analysis methods needs to be established according to the physicochemical properties and the synthesis process of the medicine.
Disclosure of Invention
The invention relates to an analysis method of a corticosteroid bulk drug, in particular to a method for measuring related substances of fluticasone furoate.
The technical scheme of the invention is as follows:
a method for detecting the content of fluticasone furoate and related substances is characterized by comprising the following steps: octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, gradient elution is carried out according to the following table,
| time (minutes) | Mobile phase A | Mobile phase B |
| 0.0 | A1 | B1 |
| 28.0-30.0 | A2 | B2 |
| 31.0-32.0 | A2 | B2 |
Wherein, A1-58%, A2-28-32%; 38-42% of B1 and 68-72% of B2.
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of: octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, and gradient elution is carried out according to the following table:
| time (minutes) | Mobile phase A | Mobile phase B |
| 0.0 | A1 | B1 |
| 28.0-30.0 | A2 | B2 |
| 31.0-32.0 | A2 | B2 |
| 32.1-32.5 | A1 | B1 |
| 35.0-38.0 | A1 | B1 |
Wherein, A1-58%, A2-28-32%; 38-42% of B1 and 68-72% of B2.
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of: octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, gradient elution is carried out according to the following table,
| time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0 | 60 | 40 |
| 30.0 | 30 | 70 |
| 32.0 | 30 | 70 |
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of:
octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, and gradient elution is carried out according to the following table:
| time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 60 | 40 |
| 30.0 | 30 | 70 |
| 32.0 | 30 | 70 |
| 32.1 | 60 | 40 |
| 35.0 | 60 | 40 |
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of: the acid in the mobile phase A and the mobile phase B is selected from trifluoroacetic acid, phosphoric acid or perchloric acid.
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of: the acid is trifluoroacetic acid.
The detection method of the content of the fluticasone furoate and related substances is characterized by comprising the following steps of: the mobile phase A is a 0.1% acid solution, and the mobile phase B is an acetonitrile solution containing 0.05% acid.
The concentration of the trifluoroacetic acid solution in the mobile phase A is 0.1%.
The concentration of the trifluoroacetic acid solution in the mobile phase B is 0.05%.
The method for detecting the content of the fluticasone furoate and related substances has the column temperature of 30-40 ℃.
The column temperature of the method for detecting the content of the furoic acid fluticasone and related substances is 35 ℃.
The flow rate of the detection method for the content of the fluticasone furoate and related substances is 1ml/min to 2.5 ml/min.
The flow rate of the method for detecting the content of the fluticasone furoate and related substances is 2 ml/min.
According to the detection method of the content of the fluticasone furoate and related substances, the detection wavelength is 245 nm.
A method for detecting the content of fluticasone furoate and related substances is used for detecting the raw material drug of fluticasone furoate.
A method for detecting the content of furoic acid fluticasone and related substances is used for detecting the medicinal preparation containing furoic acid fluticasone.
Compared with the prior art, the technical scheme of the application has the following advantages:
the method can effectively separate and detect the process impurities and the degradation impurities of the product, and the specificity and the sensitivity meet the requirements; effectively control the level of related substances of the product and ensure the safety of medication.
Drawings
FIG. 1 is a HPLC chart of inventive example 1
FIG. 2 is a HPLC chart of inventive example 2
Detailed Description
The invention will now be further described by way of the following examples, which are not intended to limit the scope of the invention in any way. It will be understood by those skilled in the art that equivalent substitutions for the technical features of the present invention, or corresponding modifications, can be made within the scope of the present invention.
Example 1
System suitability test
Taking FFZ2 reference substances, FFZ3 reference substances, FFZ6 reference substances, FFZ14 reference substances, FFZ1 reference substances, FFZ11 reference substances, FFZ12 reference substances, FFZ17 reference substances, FFZ5 reference substances, FFZ15 reference substances and FFZ16 reference substances in proper amount, precisely weighing and dissolving to obtain a mixed impurity reference substance, fixing the volume to the concentration of 1 mu g/ml, and taking fluticasone furoate reference substances to prepare 1mg/ml serving as a system applicability solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.1% trifluoroacetic acid solution;
mobile phase B: 0.05% trifluoroacetic acid in acetonitrile; the elution gradient is given in the following table,
the column temperature was 35 ℃; the flow rate was 2ml per minute; the detection wavelength is 245nm
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 60 | 40 |
| 30.0 | 30 | 70 |
| 32.0 | 30 | 70 |
| 32.1 | 60 | 40 |
| 35.0 | 60 | 40 |
The test results are shown in the attached figure 1, and the specific data are shown in the table 1:
TABLE 1 System suitability test results
Example 2
Taking a proper amount of a furoic acid fluticasone sample of FF021 batch, adding acetonitrile-water (50:50) to dissolve the furoic acid fluticasone sample to prepare a solution of 1mg/ml, and using the solution as a test sample solution; taking 1ml of the test solution, placing the test solution in a measuring flask of 100ml, adding methanol for dilution, fixing the volume to a scale, and shaking up to be used as a control solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.1% trifluoroacetic acid solution;
mobile phase B: 0.05% trifluoroacetic acid in acetonitrile; the elution gradient is given in the following table,
the column temperature was 38 ℃; flow rate was 1.5ml per minute; the detection wavelength is 245nm
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 60 | 40 |
| 30.0 | 30 | 70 |
| 32.0 | 30 | 70 |
| 32.1 | 60 | 40 |
| 35.0 | 60 | 40 |
The test results are shown in the attached figure 2, and only 4 impurities exist in the batch of samples, and the test results are shown in the table 2:
TABLE 2 test results of the samples of example 2
Example 3
System suitability test
Taking FFZ2 reference substances, FFZ3 reference substances, FFZ6 reference substances, FFZ14 reference substances, FFZ1 reference substances, FFZ11 reference substances, FFZ12 reference substances, FFZ17 reference substances, FFZ5 reference substances, FFZ15 reference substances and FFZ16 reference substances in proper amount, precisely weighing and dissolving to obtain a mixed impurity reference substance, fixing the volume to the concentration of 1 mu g/ml, and taking fluticasone furoate reference substances to prepare 1mg/ml serving as a system applicability solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.1% trifluoroacetic acid solution;
mobile phase B: 0.05% trifluoroacetic acid in acetonitrile; the elution gradient is given in the following table,
the column temperature is 30 ℃; flow rate was 1.5ml per minute; the detection wavelength is 245nm
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 58 | 42 |
| 30.0 | 28 | 72 |
| 32.0 | 28 | 72 |
| 32.1 | 58 | 42 |
| 35.0 | 58 | 42 |
The specific data of the test results are shown in Table 3:
TABLE 3 System suitability test results
Example 4
System suitability test
Taking FFZ2 reference substances, FFZ3 reference substances, FFZ6 reference substances, FFZ14 reference substances, FFZ1 reference substances, FFZ11 reference substances, FFZ12 reference substances, FFZ17 reference substances, FFZ5 reference substances, FFZ15 reference substances and FFZ16 reference substances in proper amount, precisely weighing and dissolving to obtain a mixed impurity reference substance, fixing the volume to the concentration of 1 mu g/ml, and taking fluticasone furoate reference substances to prepare 1mg/ml serving as a system applicability solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.1% trifluoroacetic acid solution;
mobile phase B: 0.05% trifluoroacetic acid in acetonitrile; the elution gradient is given in the following table,
the column temperature was 40 ℃; flow rate was 1.5ml per minute; the detection wavelength is 245nm
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 62 | 38 |
| 30.0 | 32 | 68 |
| 32.0 | 32 | 68 |
| 32.1 | 62 | 38 |
| 35.0 | 62 | 38 |
The specific data of the test results are shown in Table 4:
TABLE 4 System suitability test results
Example 5
System suitability test
Taking FFZ2 reference substances, FFZ3 reference substances, FFZ6 reference substances, FFZ14 reference substances, FFZ1 reference substances, FFZ11 reference substances, FFZ12 reference substances, FFZ17 reference substances, FFZ5 reference substances, FFZ15 reference substances and FFZ16 reference substances in proper amount, precisely weighing and dissolving to obtain a mixed impurity reference substance, fixing the volume to the concentration of 1 mu g/ml, and taking fluticasone furoate reference substances to prepare 1mg/ml serving as a system applicability solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.12% phosphoric acid solution;
mobile phase B: 0.07% phosphoric acid in acetonitrile; the elution gradient is given in the following table,
the column temperature is 30 ℃; flow rate was 1.5ml per minute; the detection wavelength is 245nm
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.0 | 58 | 42 |
| 30.0 | 28 | 72 |
| 32.0 | 28 | 72 |
| 32.1 | 58 | 42 |
| 35.0 | 58 | 42 |
The specific data of the test results are shown in table 5:
TABLE 5 System suitability test results
Example 6
System suitability test
Taking FFZ2 reference substances, FFZ3 reference substances, FFZ6 reference substances, FFZ14 reference substances, FFZ1 reference substances, FFZ11 reference substances, FFZ12 reference substances, FFZ17 reference substances, FFZ5 reference substances, FFZ15 reference substances and FFZ16 reference substances in proper amount, precisely weighing and dissolving to obtain a mixed impurity reference substance, fixing the volume to the concentration of 1 mu g/ml, and taking fluticasone furoate reference substances to prepare 1mg/ml serving as a system applicability solution.
Blank solution: acetonitrile-water (50: 50);
sample introduction by high performance liquid chromatography
Chromatographic column using octadecylsilane chemically bonded silica as filler (Zorbax SB-C18, 150mm × 4.6.6 mm, 3.5 μm)
Mobile phase A: 0.08% perchloric acid solution;
mobile phase B: 0.03% perchloric acid in acetonitrile; the elution gradient is given in the following table,
the column temperature was 40 ℃; flow rate was 1.5ml per minute; the detection wavelength is 245nm
The specific data of the test results are shown in Table 6:
TABLE 6 System suitability test results
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A method for detecting the content of fluticasone furoate and related substances is characterized by comprising the following steps:
octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, gradient elution is carried out according to the following table,
Wherein, A1-58%, A2-28-32%; 38-42% of B1 and 68-72% of B2.
2. The method for detecting the content of fluticasone furoate and related substances according to claim 1, wherein the method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, and gradient elution is carried out according to the following table:
Wherein, A1-58%, A2-28-32%; 38-42% of B1 and 68-72% of B2.
3. The method for detecting the content of fluticasone furoate and related substances according to claim 1, wherein the method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, gradient elution is carried out according to the following table,
4. the method for detecting the content of fluticasone furoate and related substances according to claim 1, wherein the method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filling agent, an ultraviolet detector is adopted, the detection wavelength is 240nm-255nm, 0.08% -0.12% acid solution is used as a mobile phase A, acetonitrile solution containing 0.03% -0.07% acid is used as a mobile phase B, and gradient elution is carried out according to the following table:
5. The method for detecting the content of fluticasone furoate and related substances according to any one of claims 1 to 4, wherein the method comprises the following steps: the acid in the mobile phase A and the mobile phase B is selected from trifluoroacetic acid, phosphoric acid or perchloric acid.
6. The method for detecting the content of fluticasone furoate and related substances according to claim 5, wherein the method comprises the following steps: the acid is trifluoroacetic acid.
7. The method for detecting the content of fluticasone furoate and related substances according to any one of claims 1 to 4 and 6, wherein the method comprises the following steps: the mobile phase A is a 0.1% acid solution, and the mobile phase B is an acetonitrile solution containing 0.05% acid.
8. The method for detecting the content of fluticasone furoate and related substances according to claims 1-4, wherein the method comprises the following steps: the detection wavelength was 245 nm.
9. The method for detecting the content of fluticasone furoate and related substances according to claims 1-4, wherein the method comprises the following steps: the column temperature is 30-40 ℃.
10. The method for detecting the content of fluticasone furoate and related substances according to claims 1-4, wherein the method comprises the following steps: the flow rate is 1 ml/min-2.5 ml/min.
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