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Method for detecting 2,2,6,6-tetramethylpiperidinooxy with high performance liquid chromatography-mass spectrometry

A technology of tetramethylpiperidine and nitrogen oxides, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of weak ultraviolet absorption, low sensitivity, and inaccurate detection results, and achieve accurate detection results, high sensitivity, Simple operation effect

Inactive Publication Date: 2019-04-16
CHANGZHOU HEQUAN PHARMA CO LTD
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Problems solved by technology

There is no relevant detection method for this compound reported in the literature at present. Since 2,2,6,6-tetramethylpiperidine nitrogen oxide has only a very weak ultraviolet absorption, a high-performance liquid phase-ultraviolet detector is used. Due to the condition defect, the detection Inaccurate results, low sensitivity, and great limitations in quantitative detection

Method used

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  • Method for detecting 2,2,6,6-tetramethylpiperidinooxy with high performance liquid chromatography-mass spectrometry
  • Method for detecting 2,2,6,6-tetramethylpiperidinooxy with high performance liquid chromatography-mass spectrometry
  • Method for detecting 2,2,6,6-tetramethylpiperidinooxy with high performance liquid chromatography-mass spectrometry

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Embodiment 1

[0030] 1. Instruments and Reagents

[0031] instrument:

[0032] HPLC-MS: Agilent 6525B HPLC-Quadrupole-TOF Mass Spectrometer Parts per million Analytical Balance: Mettler Toledo XSE205DU

[0033] Reagent:

[0034] Water: Millipore ultrapure water

[0035] Acetonitrile: Merck chromatography pure

[0036] Formic acid: J&K chromatographically pure

[0037] Sodium ascorbate: Damas-beta analytically pure

[0038] 2,2,6,6-tetramethylpiperidine nitrogen oxide: Aldrich, content 98%

[0039] 2. Detection conditions of high performance liquid chromatography-mass spectrometry

[0040] High performance liquid chromatography conditions:

[0041] Chromatographic column: Waters Xbridge Phenyl (150×4.6mm, 3.5μm);

[0042] Mobile phase A: aqueous solution containing 0.1% formic acid by volume fraction;

[0043] Mobile phase B: acetonitrile solution containing 0.1% formic acid by volume fraction;

[0044] Flow rate: 1.0mL / min;

[0045] Column temperature: 40°C;

[0046] Injection v...

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Abstract

The invention discloses a method for detecting 2,2,6,6-tetramethylpiperidinooxy with high performance liquid chromatography-mass spectrometry. The method comprises the steps that 1, a test solution and a reference stock solution is prepared; 2, the test solution and the reference stock solution with a certain concentration gradient are subjected to sample introduction, a high performance liquid chromatograph mass spectrometer is used for detecting and recording a chromatogram; and 3, linear regression analysis is performed on the mass concentration of the reference stock solution and chromatogram peak area, a regression equation and correlation coefficients are obtained, and a standard curve is manufactured; and the peak area of 2,2,6,6-tetramethylpiperidinooxy in the chromatogram of the test solution is utilized to calculate the content of 2,2,6,6-tetramethylpiperidinooxy by an external standard method. The method provided by the invention is the first method for detecting 2,2,6,6-tetramethylpiperidinooxy developed in the field. The method has accurate detection result, high sensitivity, good stability, and low detection limit, and totally meets detection requirements for genotoxic impurities in the field.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting the content of 2,2,6,6-tetramethylpiperidine nitrogen oxides in drugs by liquid mass spectrometry. Background technique [0002] 2,2,6,6-Tetramethylpiperidine nitrogen oxide, chemical name 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO), is a typical piperidine nitrogen oxide free radical, in It is widely used in chemistry, biology, food industry, agriculture and other fields. It is mainly used as a catalyst to synthesize drugs and pharmaceutical intermediates. In organic synthesis, 2,2,6,6-tetramethylpiperidine nitrogen oxide can catalyze green oxidants such as hydrogen peroxide, oxygen and sodium hypochlorite to quantitatively oxidize primary and secondary alcohols to aldehydes and ketones under mild conditions. The reaction has high selectivity, the primary alcohol is oxidized to aldehyde, no longer oxidized to carboxylic acid, the secondary alcohol ...

Claims

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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 胡研黄勤琴陈伊杰蒋竞赵初芒
Owner CHANGZHOU HEQUAN PHARMA CO LTD
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