Method for analytical separation sodium ibandronate and impurities thereof by utilizing high performance liquid chromatography (HPLC)

A technology for analysis and separation of ibandronate sodium, applied in the field of analysis of ibandronate sodium raw materials and preparations, can solve the problems of increased detection cost, many interference factors, low accuracy, etc., and achieve reduced detection cost, accurate High accuracy, high accuracy effect

Inactive Publication Date: 2013-06-05
CHENGDU EASTON BIOPHARMACEUTICALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both of these two methods of determination have the disadvantages of cumbersome operation, many interference factors, and low accuracy; at the same time, both methods require a large number of samples, which greatly increases the detection cost

Method used

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  • Method for analytical separation sodium ibandronate and impurities thereof by utilizing high performance liquid chromatography (HPLC)
  • Method for analytical separation sodium ibandronate and impurities thereof by utilizing high performance liquid chromatography (HPLC)
  • Method for analytical separation sodium ibandronate and impurities thereof by utilizing high performance liquid chromatography (HPLC)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Instruments and Conditions

[0084] High performance liquid chromatography: Shimadzu: LC-20ATSPD-M20A

[0085] Chromatographic column: C18 (150×4.6mm)

[0086] Mobile phase: 0.02mol / L potassium dihydrogen phosphate (0.01% EDTA): acetonitrile=97:3

[0087] Flow rate: 1.2mL / min

[0088] Detection wavelength: 200nm

[0089] Injection volume: 20μL

[0090] Experimental steps:

[0091] Take ibandronate sodium impurity I: 10.2mg, impurity II: 9.9mg and ibandronate sodium: 10.3mg, put them in three 10mL measuring bottles respectively, add mobile phase to dissolve and dilute to the mark, as the reference substance solution, Then accurately weigh ibandronate sodium raw material: 10.5mg, impurity I: 10.0mg, impurity II: 10.7mg and place in the same 10ml measuring bottle, add mobile phase to dissolve and dilute to the mark, as the test solution. Get above-mentioned solution and carry out high performance liquid chromatography analysis according to above-mentioned chromatogra...

Embodiment 2

[0094] Instruments and Conditions

[0095] High performance liquid chromatography: Agilent1200

[0096] Chromatographic column: C8 (200×4.6mm)

[0097] Mobile phase: 0.01mol / L sodium dihydrogen phosphate (0.01%EDTA):methanol=98:2

[0098] Flow rate: 0.8mL / min

[0099] Detection wavelength: 195nm

[0100] Injection volume: 10μL

[0101] Experimental procedure

[0102] The preparation method of need testing solution is with embodiment 1.

[0103] Get need testing solution, carry out HPLC analysis by above-mentioned chromatographic condition, record chromatogram, the result sees attached Figure 5 . In the figure, peak No. 1 is the chromatographic peak of impurity II, peak No. 2 is the chromatographic peak of ibandronic acid, and peak No. 3 is the chromatographic peak of impurity I. It can be seen that under this condition, ibandronic acid and two of them All impurities can be effectively separated, and the retention time of ibandronic acid is about 12.3min.

Embodiment 3

[0105] Instruments and Conditions

[0106] High performance liquid chromatography: Agilent1200

[0107] Chromatographic column: C18 (250×4.6mm)

[0108] Mobile phase: 0.05mol / L potassium dihydrogen phosphate (0.01% EDTA):methanol=94:6

[0109] Flow rate: 1.0mL / min

[0110] Detection wavelength: 205nm

[0111] Injection volume: 50μL

[0112] Experimental procedure

[0113] The preparation method of need testing solution is with embodiment 1.

[0114] Get need testing solution, carry out HPLC analysis by above-mentioned chromatographic condition, record chromatogram, the result sees attached Image 6 .

[0115] In the figure, peak No. 1 is the chromatographic peak of impurity II, peak No. 2 is the chromatographic peak of ibandronic acid, and peak No. 3 is the chromatographic peak of impurity I. It can be seen that under this condition, ibandronic acid and two of them All impurities can be separated effectively, and the retention time of ibandronic acid is about 8.3min. ...

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Abstract

The invention discloses a high performance liquid chromatography (HPLC), in particular to a method for analyzing sodium ibandronate and pereparation by utilizing the HPLC. Octyl or octadecyl silicane bonded silica gel is adopted as a chromatographic column of filler, methyl alcohol-phosphate buffered saline or acetonitrile-phosphate buffered saline is used as a mobile phase for chromatographic column separation, and an ultraviolet detector is used for detecting the sodium ibandronate and the impurities of the sodium ibandronat. With the method, effective separation of the sodium ibandronat, the impurities I and the impurities II can be conducted well, the contents of the sodium ibandronat can be measured accurately, and quality of sodium ibandronat products can be guaranteed well. The method has the advantages of being strong in specificity, simple in operation and high in accuracy.

Description

technical field [0001] The invention discloses an HPLC method, in particular to an analysis method for ibandronate sodium raw materials and preparations. Background technique [0002] Sodium ibandronate is the main drug for the prevention and treatment of various metabolic bone diseases and osteoporosis mainly destroying cellular bone resorption. Its structural formula is [0003] [0004] Sodium ibandronate [0005] The chemical name is 1-hydroxy-3-(N-methyl-pentylamino)-propylene diphosphonic acid monosodium salt monohydrate. During the synthesis of this compound, there are several important intermediates or degradation products that may affect the purity and quality of the drug due to incomplete removal. In the synthetic process of sodium ibandronate, it is mainly necessary to control the intermediate impurity I (3-N-methyl-N-pentylaminopropionic acid) and the degradation product impurity II of the finished product (1-hydroxyl-3-(N- Amylamino)-propylene diphosphonic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 王颖胡同军
Owner CHENGDU EASTON BIOPHARMACEUTICALS CO LTD
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