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Method for detecting hydrazine hydrate in medicine

A detection method and technology of hydrazine hydrate, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as the need to improve accuracy and stability, and achieve the effects of good applicability and reliability, excellent linearity, and improved resolution

Active Publication Date: 2021-08-24
广州国标检验检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the accuracy and stability of this method still need to be improved

Method used

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  • Method for detecting hydrazine hydrate in medicine
  • Method for detecting hydrazine hydrate in medicine
  • Method for detecting hydrazine hydrate in medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Take 0.5g of p-dimethylaminobenzaldehyde, accurately weigh it, put it in a 25ml volumetric flask, add glacial acetic acid-ethanol (1:9) solution to dissolve to constant volume, and obtain a derivative reagent;

[0042] (2) Take an appropriate amount of hydrazine standard solution in a 10ml volumetric flask, add water to dilute to the mark, shake well, and dilute with ethanol to prepare standards with hydrazine hydrate concentrations of 18.66~932.81 ng / ml (hydrazine hydrate limit percentage: 5~250%) curve solution;

[0043] (3) Take 50 mg of raw drug powder (oseltamivir) and add ethanol to dissolve it, use a 10 ml volumetric flask to obtain the test solution, take 50 mg of raw drug powder and add it to the reference solution (373.13 ng / mL) bottle to constant volume to obtain the spiked solution;

[0044] (4) Take ethanol solvent, standard curve solution, test solution and spiked solution respectively and add derivatization reagents for derivatization reaction, sonic...

Embodiment 2

[0076] Referring to the detection method of Example 1, the volume ratio is 1:19, the only difference is to adjust the temperature and time of the derivatization reaction, detect the peak area of ​​the 100% limit reference solution (373.13ng / mL), and repeat the measurement 3 times to get the average value. The experimental parameters and results are shown in Table 5 below.

[0077] The results show that the derivatization can be completed when the derivatization temperature is 25℃ and the derivatization time is 40~60min, especially when the sonication is 40min, the derivatization efficiency is the highest and the derivative product is the most stable. However, when the derivatization temperature was 50°C, the derivative products in the system were unstable, and the peak area dropped sharply, which may have introduced interfering substances to affect the measurement results.

[0078] table 5

[0079]

Embodiment 3

[0081] Referring to the detection method of Example 1, the volume ratio is 1:19, the only difference is that the solvent of the derivatization reagent is adjusted, the recovery rate of the spiked solution is detected, and the measurement is repeated 6 times. The experimental parameters and results are shown in Table 6 below.

[0082] The results showed that the use of methanol as a solvent for the derivatization reagent would cause great interference to the system, and the use of aqueous solution would affect the solubility of the test sample, which were not suitable for the detection of hydrazine hydrate in drugs. In the glacial acetic acid-ethanol (1:9) system, the recovery rate of the spiked solution was the highest and the stability was the strongest, meeting the detection requirements.

[0083] Table 6

[0084]

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Abstract

The invention belongs to the technical field of medicine detection, and particularly discloses a method for detecting hydrazine hydrate in a medicine. The detection method provided by the invention has excellent linearity, detection limit, specificity and accuracy, is good in applicability and reliability, and accords with drug detection regulations; in addition, appropriate dosage and reaction conditions of the derivatization reagent are tested, so that the derivatization efficiency and the stability of a derivative product are improved; parameters of liquid phase and mass spectrum conditions are determined, and the detection sensitivity of derivative products and the separation degree of interference peaks are improved.

Description

technical field [0001] The invention belongs to the technical field of drug detection, in particular to a method for detecting hydrazine hydrate in drugs. Background technique [0002] Hydrazine hydrate is a genotoxic impurity in pharmaceuticals, and its quantitative detection is very important for the quality control of pharmaceuticals. Due to the instability of hydrazine hydrate, there are many interference factors in the direct detection. At present, the detection method of hydrazine hydrate in drugs mainly adopts derivatization liquid chromatography, but there are still problems of long analysis time and poor sensitivity. Aiming at this problem, patent CN108459107A discloses a method for determining residual hydrazine hydrate in medicines by liquid chromatography-mass spectrometry. However, the accuracy and stability of this method still need to be improved. Contents of the invention [0003] In order to overcome the shortcomings and deficiencies of the above-mention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8675G01N2030/324
Inventor 郑传奇邱全玉左仕深曹丹邵广志梁雨昕蒋杰
Owner 广州国标检验检测有限公司
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