Method for detecting hydroxylamine hydrochloride in azilsartan

A detection method, the technology of hydroxylamine hydrochloride, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of non-conforming recovery rate, difficult recovery rate meeting the standard, and large matrix influence

Active Publication Date: 2020-10-30
珠海润都制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when used for the detection of hydroxylamine hydrochloride in azilsartan, the matrix has a great influence, and the recovery rate does not meet the standard
In addition, the inventor has also studied other mobile phases, such as using mobile phase A to be 0.05% formic acid aqueous solution, fluidity B to be 0.05% formic acid acetonitrile solution, adopting benzaldehyde to derivatize hydroxylamine hydrochloride, and adopting various fluidity ratios Carry out research, but the influence of the matrix is ​​large, and the recovery rate is difficult to meet the standard

Method used

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  • Method for detecting hydroxylamine hydrochloride in azilsartan
  • Method for detecting hydroxylamine hydrochloride in azilsartan
  • Method for detecting hydroxylamine hydrochloride in azilsartan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Embodiment 1 detection method

[0078] Instrument conditions and reagents

[0079] Instrument: high performance liquid chromatography equipped with ultraviolet detector, electronic analytical balance.

[0080] Chromatographic column: use octadecylsilane bonded silica gel as filler (such as: Agilent ZORBAX SB-C18 4.6×150mm, 5.0µm or a column with equivalent performance);

[0081] Flow rate: 0.8ml / min; Detection wavelength: 254nm;

[0082] Injection volume: 10μl; Column temperature: 40°C;

[0083] Sample tray temperature: 8°C;

[0084] Mobile phase A: 10mmol / L ammonium formate solution (containing 0.1% formic acid);

[0085] Mobile phase B: acetonitrile;

[0086] The gradient table is shown in Table 1.

[0087] (1) Solution preparation:

[0088] Derivative medium: 0.25mol / L sodium hydroxide methanol solution (take about 2g of sodium hydroxide, add 200ml of methanol to dissolve)

[0089] Derivative: 0.5mg / ml benzaldehyde methanol solution (take about 50mg benzaldeh...

Embodiment 2

[0105] Embodiment 2 System Applicability

[0106] System suitability is realized by measuring the S / N value of hydroxylamine hydrochloride in the sensitivity solution and the RSD of the peak area of ​​hydroxylamine hydrochloride in the standard solution. It is required that the S / N value of hydroxylamine hydrochloride in the sensitivity solution should be ≥10; 6, the RSD of the peak area of ​​hydroxylamine hydrochloride in the standard solution should not be greater than 10.0%.

[0107] The solution was prepared, and samples were injected according to the conditions of Example 1. The test results are shown in Table 6.

[0108]

Embodiment 3

[0109] Example 3 specificity

[0110] The specificity of the method is achieved by determining the non-interference of the blank solution to the detection; the resolution between hydroxylamine hydrochloride and adjacent peaks in the selective solution. It is required that the blank solution should not interfere with the detection; the separation between hydroxylamine hydrochloride and adjacent peaks in the selective solution should not be less than 1.5.

[0111] The solution was prepared, and samples were injected according to the conditions of Example 1. The test results are shown in Table 7.

[0112]

[0113] Conclusion: The blank solution has no interference to the detection; the resolution between hydroxylamine hydrochloride and adjacent peaks in the selective solution is 2.1, which meets the standard.

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Abstract

The invention provides a method for detecting the content of hydroxylamine hydrochloride in azilsartan. According to the method, hydroxylamine is subjected to derivatization treatment by adopting benzaldehyde, octadecylsilane chemically bonded silica is used as a filler of a chromatographic column, a mobile phase A is a 10mmol/L ammonium formate solution (containing 0.1% of formic acid), a mobilephase B is acetonitrile, gradient elution is adopted, a sample does not need to be specially treated, and matrix influence is avoided. According to the detection method, azilsartan is adopted as a test sample, and the system applicability, specificity, detection limit, durability and other items prove that azilsartan meets related requirements.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting the impurity content of hydroxylamine hydrochloride in a sample by using high-performance liquid chromatography, and more specifically, detecting the impurity content of hydroxylamine hydrochloride in azilsartan by using high-performance liquid chromatography. Background technique [0002] Hydroxylamine hydrochloride (molecular formula NH2OH·HCl, CAS: 5470-11-1) is a material used in the synthesis process of azilsartan (molecular formula C25H20N4O5, CAS: 147403-03-0), document (Synthesis of Azilsartan and ItsSelected Potential Impurities [J]. Journal of Heterocyclic Chemistry, 2013, 50(4).) reported that azilsartan was synthesized by hydroxylamine hydrochloride, so hydroxylamine hydrochloride may remain in the finished product of azilsartan. [0003] At present, there is no detection method for the content of hydroxylamine hydrochloride in azilsartan ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 谢金昌顾琼汤伟彬
Owner 珠海润都制药股份有限公司
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