CN102116765A - Method for measuring related substance of minodronate intermediate by high performance liquid chromatography - Google Patents
Method for measuring related substance of minodronate intermediate by high performance liquid chromatography Download PDFInfo
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- CN102116765A CN102116765A CN2009102443836A CN200910244383A CN102116765A CN 102116765 A CN102116765 A CN 102116765A CN 2009102443836 A CN2009102443836 A CN 2009102443836A CN 200910244383 A CN200910244383 A CN 200910244383A CN 102116765 A CN102116765 A CN 102116765A
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- acid intermediate
- minodronic acid
- buffer salt
- related substance
- chromatographic column
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Abstract
The invention discloses a method for separating, analyzing and measuring a related substance of a minodronate intermediate. In the method, octylsilane bonded silica gel is used as a filler chromatographic column and anion buffer salt solution-organic modifier is used as a mobile phase for separating the related substance of the minodronate intermediate.
Description
Technical field
The invention belongs to and relate to a kind of high performance liquid chromatography method for separating and analyzing, particularly a kind of method with high performance liquid chromatography compartment analysis minodronic acid intermediate related substance.
Background technology
Minodronic acid is a kind of medicine for the treatment of osteoporosis, its intermediate structural formula:
The HPLC detection method of this compound does not have bibliographical information at present, does not apply for a patent yet.
This law is effectively carried out purity analysis to the minodronic acid intermediate, and common chromatographic column C is adopted in this test
8Chromatographic column has realized the mensuration of minodronic acid intermediate related substance fast and accurately, thereby realized the control of minodronic acid intermediate impurity, guaranteed the quality controllable of minodronic acid intermediate, had important practical significance aspect the quality control of the synthetic and preparation process of minodronic acid.
Summary of the invention
The object of the present invention is to provide a kind of efficient liquid-phase chromatography method of compartment analysis minodronic acid intermediate related substance, thereby realize quality control the minodronic acid intermediate.
The applicant finds, with octyl silane group silica gel chromatographic column, is moving phase with negative ion to buffer salt solution-organic modifiers, can realize separating and analyzing of minodronic acid intermediate and its related substance, thereby can accurately control the quality of minodronic acid intermediate and preparation thereof.
The said method of the present invention with high performance liquid chromatography compartment analysis minodronic acid intermediate, wherein:
Chromatographic column is selected octyl silane group silica gel for use, and specification is 250mm * 4.6mm, 5 μ m.
The organic modifiers that the present invention adopts is selected from acetonitrile, methyl alcohol, and most preferred organic modifiers is a methyl alcohol.
Moving phase: sodium lauryl sulfate buffer (pH 2.5)-organic modifiers.
Buffer salt is selected from potassium dihydrogen phosphate, and sodium dihydrogen phosphate is preferably sodium dihydrogen phosphate.
Organic modifiers is selected from acetonitrile, methyl alcohol, is preferably methyl alcohol.
The volume ratio of sodium lauryl sulfate buffer in the moving phase of the inventive method-organic modifiers mixed solution is 50: 50.
The pH value of the sodium lauryl sulfate buffer of the inventive method is 2.5.
Method for separating and analyzing of the present invention, can realize in accordance with the following methods:
(1) it is an amount of to take by weighing minodronic acid intermediate sample, uses the moving phase sample dissolution, is mixed with the sample solution that every 1ml contains minodronic acid intermediate 0.2mg～2mg approximately.
(2) flow rate of mobile phase being set is 0.8～1.2ml/min, and the detection wavelength is 220nm.
(3) the sample solution 5-40 μ l that gets step (1) injects liquid chromatograph, finishes the separation and the analysis of minodronic acid intermediate.
Wherein:
High performance liquid chromatograph: Tianjin, island: LC-10ATvp, SPD-10Avp, SCL-10Avp, DGU-12A
Chromatographic column: octyl silane group silica gel is the chromatographic column 250mm * 4.6mm of filling agent, 5 μ m
Moving phase: sodium lauryl sulfate buffer (regulating the pH value with phosphoric acid,diluted is 2.5)-methyl alcohol 50: 50
Flow velocity: 1.0ml/min
Detect wavelength: 220nm
Column temperature: room temperature
Sampling volume: 10 μ l
The present invention can effectively measure the related substance of minodronic acid intermediate, the method simple and fast, and the sensitivity for analysis height, the result is accurately and reliably.Can be used for the quality control of minodronic acid intermediate, guarantee the quality controllable of bulk drug and preparation.
Description of drawings
Fig. 1 embodiment 1, sodium lauryl sulfate buffer (regulating the pH value with phosphoric acid,diluted is 2.5)-methyl alcohol (50: 50) minodronic acid intermediate and related substance biased sample high-efficient liquid phase chromatogram
Fig. 2 embodiment 2, sodium lauryl sulfate buffer (regulating the pH value with phosphoric acid,diluted is 2.5)-methyl alcohol (50: 50) minodronic acid intermediate high-efficient liquid phase chromatogram
Embodiment: following examples are used for further understanding the present invention, but are not limited to the scope of this enforcement
Embodiment 1
Instrument and condition
High performance liquid chromatograph: day island proper Tianjin: LC-10ATvp, SPD-10Avp
Chromatographic column: octyl silane group silica gel chromatographic column (250mm * 4.6mm, 5 μ m)
Moving phase: sodium lauryl sulfate buffer (regulating the pH value with phosphoric acid,diluted is 2.5)-methyl alcohol (50: 50)
Flow velocity: 1.0ml/min
Detect wavelength: 220nm
Column temperature: room temperature
Sampling volume: 10 μ l
Experimental procedure
Take by weighing minodronic acid intermediate 10mg, intermediate compound I 2mg places the 10ml volumetric flask, adds the moving phase dissolving and is diluted to scale, shakes up, as need testing solution.Get need testing solution, carry out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, the record chromatogram the results are shown in accompanying drawing 1.
Retention time is that 9.5 minutes chromatographic peak is the chromatographic peak of minodronic acid intermediate among Fig. 1, and retention time is the chromatographic peak that 19.9 minutes chromatographic peaks are related substance I.Chromatogram shows that the minodronic acid intermediate can be issued to good separating at same chromatographic condition with its intermediate and impurity.
Instrument and condition
High performance liquid chromatograph: day island proper Tianjin: LC-10TAvp, SPD-10Avp
Chromatographic column: octyl silane group silica gel chromatographic column (250mm * 4.6mm, 5 μ m)
Moving phase: sodium lauryl sulfate buffer (regulating the pH value with phosphoric acid,diluted is 2.5)-methyl alcohol (50: 50)
Flow velocity: 1.0ml/min
Detect wavelength: 220nm
Column temperature: room temperature
Sampling volume: 10 μ l
Experimental procedure
Take by weighing minodronic acid intermediate 10mg, place the 10ml volumetric flask, add the moving phase dissolving and be diluted to scale, shake up, as need testing solution.Get need testing solution, carry out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, the record chromatogram the results are shown in accompanying drawing 2.
Claims (10)
1. the method for a high performance liquid chromatography compartment analysis minodronic acid intermediate related substance, it is characterized in that adopting octyl silane group silica gel is the chromatographic column of filling agent, is moving phase with negative ion to buffer salt solution-organic modifiers.
2. method according to claim 1 is characterized in that described chromatographic column is that the chromatographic column specification that the silica-based alkane bonded silica gel of octane is a filling agent is 250mm * 4.6mm, 5 μ m.
3. method according to claim 1 is characterized in that described negative ion is a lauryl sodium sulfate to reagent.
4. method according to claim 1 is characterized in that described buffer salt is selected from potassium dihydrogen phosphate, sodium dihydrogen phosphate.
5. method according to claim 4 is characterized in that described buffer salt is a sodium dihydrogen phosphate.
6. method according to claim 1 is characterized in that described organic modifiers is selected from acetonitrile, methyl alcohol.
7. method according to claim 6 is characterized in that described organic modifiers is a methyl alcohol.
8. method according to claim 1, the pH value that it is characterized in that described buffer salt solution is 2.5.
9. method according to claim 1 is characterized in that negative ion in the moving phase is 50: 50 to the volume ratio of buffer salt solution and organic modifiers.
10. method according to claim 1 is characterized in that may further comprise the steps:
(1) it is an amount of to take by weighing minodronic acid intermediate sample, uses the moving phase sample dissolution, is mixed with the solution that every 1ml contains minodronic acid intermediate sample 0.2～2mg approximately.
(2) flow rate of mobile phase being set is 0.8～1.2ml/min, and the detection wavelength is 220nm.
(3) the sample solution 5-40 μ l that gets step (1) injects liquid chromatograph, finishes the separation and the analysis of minodronic acid intermediate and related substance thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102443836A CN102116765A (en) | 2009-12-30 | 2009-12-30 | Method for measuring related substance of minodronate intermediate by high performance liquid chromatography |
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| CN2009102443836A CN102116765A (en) | 2009-12-30 | 2009-12-30 | Method for measuring related substance of minodronate intermediate by high performance liquid chromatography |
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| CN102116765A true CN102116765A (en) | 2011-07-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467027A (en) * | 2015-11-18 | 2016-04-06 | 北京万全德众医药生物技术有限公司 | A method of separating and measuring compounds related to a minodronic acid intermediate through gas chromatography |
| CN114384186A (en) * | 2022-01-21 | 2022-04-22 | 王立强 | Method for measuring content of (2E, 4E) -ethyl-4- (pyridine-2-yl imino) -2-ethyl crotonate |
-
2009
- 2009-12-30 CN CN2009102443836A patent/CN102116765A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| KATSUTOSHI NAKAMURA等: "Stabilization of minodronic acid in aqueous solution for parenteral formulation", 《INTERNATIONAL JOURNAL OF PHARMACEUTICS》 * |
| 唐克慧等: "离子交换HPLC法测定唑来膦酸的含量及有关物质", 《中国抗生素杂志》 * |
| 张晓青: "双膦酸类药物质量及其质量控制研究", 《中国优秀博硕士学位论文全文数据库(硕士)医药卫生科技辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467027A (en) * | 2015-11-18 | 2016-04-06 | 北京万全德众医药生物技术有限公司 | A method of separating and measuring compounds related to a minodronic acid intermediate through gas chromatography |
| CN105467027B (en) * | 2015-11-18 | 2021-09-21 | 北京万全德众医药生物技术有限公司 | Method for separating and measuring minodronate intermediate related substances by gas chromatography |
| CN114384186A (en) * | 2022-01-21 | 2022-04-22 | 王立强 | Method for measuring content of (2E, 4E) -ethyl-4- (pyridine-2-yl imino) -2-ethyl crotonate |
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