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Method for determining hydrazine hydrate through derived HPLC (High Performance Liquid Chromatography)

A hydrazine hydrate and derivatization technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of restricted popularization, high price, high requirements for columns, etc., and achieves good linear relationship, good specificity, no The effect of matrix interference

Inactive Publication Date: 2017-08-18
常州佳德医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The direct method is carried out with a thermal conductivity detector (TCD). Since the thermal conductivity detector is not very sensitive, the analytical sensitivity of this method is low. In addition, since hydrazine hydrate is a strong basic compound, there are also high requirements for the selection of columns.
Zhang Yu et al. used furfural derivatization-gas chromatography / mass spectrometry to determine hydrazine in surface water. Although mass spectrometry is a sensitive and versatile detector, its high price limits its popularization.
[0005] Compared with water sample analysis, the determination of residual hydrazine hydrate in APIs faces more challenges

Method used

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  • Method for determining hydrazine hydrate through derived HPLC (High Performance Liquid Chromatography)
  • Method for determining hydrazine hydrate through derived HPLC (High Performance Liquid Chromatography)
  • Method for determining hydrazine hydrate through derived HPLC (High Performance Liquid Chromatography)

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Embodiment Construction

[0022] The technical solution of the present invention will be further described below in conjunction with the accompanying drawings.

[0023] 1.1. Instruments

[0024] Shimadzu LC-20AD liquid chromatograph (including online vacuum degasser, binary gradient pump, autosampler, column oven, UV detector and Labsolution chromatography workstation) Sartorius BT125D electronic balance (Beijing Sartorius Co., Ltd.) .

[0025] 1.2. Reagents

[0026] Glacial acetic acid (99.5%), hydrazine hydrate (98%), 2-hydroxy-1-naphthaldehyde (98%), dimethylsulfoxide (99%), purified water, acetonitrile (TEDIA, chromatographically pure), trifluoroacetic acid (chromatographically pure).

[0027] 1.3. Solution preparation

[0028] 2-Hydroxy-1-naphthaldehyde (hereinafter referred to as HNA): Take 250 mg of the reagent, weigh it accurately, place it in a 50 mL volumetric flask, dilute to the mark with dimethyl sulfoxide, dissolve and shake well.

[0029] Hydrazine hydrate: Weigh 10 mg of the reagen...

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Abstract

The invention discloses a method for determining hydrazine hydrate through derived HPLC (High Performance Liquid Chromatography). The method comprises the following steps: carrying out derivatization on hydrazine by using an aldehyde ketone derivatization reagent under a water bath condition of 100 DEG C, and generating a product-hydrazone having stronger absorptivity in an ultraviolet visible zone; using a reaction solution after completing a derivatization reaction as a sample injection sample, and determining the derived product-hydrozone of the hydrazine hydrate in the ultraviolet visible zone by utilizing the HPLC and based on reversed partition chromatography, thus realizing quantitative detection on the hydrazine hydrate. Since the absorptivity of most of bulk drugs and impurities thereof in a far ultraviolet visible zone is very weak, the simple method for determining the hydrazine hydrate through pre-column derivatization HPLC is established based on the hydrazine derivatization product of the aldehyde ketone derivatization reagent. A methodology validation result shows that the method is good in specificity.

Description

technical field [0001] The invention belongs to the field of analysis and detection of crude drugs, in particular to a method for determining hydrazine hydrate in crude drugs by derivatization HPLC. Background technique [0002] As an important fine chemical raw material, hydrazine hydrate is mainly used to synthesize AC, D1PA, TSH and other foaming agents; it is also used as a cleaning agent for deoxidation and decarbonation of boilers and reactors; it is used in the production of weed control in the pesticide industry Hydrazine can be used as anti-tuberculosis and anti-diabetic drugs in the pharmaceutical industry. Hydrazine can cause toxic and side effects to the liver, kidney, blood and other systems. According to data, hydrazine may be carcinogenic; therefore, this type of compound is often easy to remain in medicines, and excessive intake may cause harm to the human body. At present, the threshold of toxicological concern (TTC) is widely used in the world to control t...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张林
Owner 常州佳德医药科技有限公司
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