A method for detecting tedizolid phosphate isomer impurities

A technology of tedizolid phosphate and a detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, unfavorable accurate quantification, and inability to meet the needs of effective and accurate quantification, and achieve accurate separation and reliable quality. control effect

Active Publication Date: 2019-09-24
NANJING YOUKE BIOLOGICAL MEDICAL RES +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, CN105085570A discloses a chromatographic column packed with octadecylsilane bonded silica gel ( XB-C18, 4.6×300nm, 5μm), 0.025mol / L ammonium bicarbonate solution-acetonitrile (95:5) and acetonitrile as mobile phase, gradient elution method to separate tedizolid phosphate and its optical isomerism in the sample However, the results show that the peak tailing is more serious (the tailing factor of tedizolid phosphate peak is 1.567), which is not conducive to accurate quantification
It can be seen that the above method either needs to use expensive instruments, or the separation condition is not ideal, and cannot meet the current demand for effective and accurate quantification of isomer impurities in tedizolid phosphate

Method used

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  • A method for detecting tedizolid phosphate isomer impurities
  • A method for detecting tedizolid phosphate isomer impurities
  • A method for detecting tedizolid phosphate isomer impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1 High performance liquid chromatography analysis of tedizolid phosphate and its isomers by phosphatase hydrolysis

[0057] 1. Selection of phosphatase hydrolysis conditions

[0058] Solution preparation:

[0059] pH9.0 buffer solution: Accurately weigh 3.1g of boric acid, put it in a 1L volumetric flask, add 500ml of water to dissolve it, and accurately add 21ml of 1mol / L NaOH solution and 10ml of 0.1mol / L MgCl 2 solution, dilute to the mark with water, shake well, and use it as a pH9.0 buffer solution.

[0060] Alkaline phosphatase solution (newly prepared for temporary use): Accurately weigh 100mg of alkaline phosphatase, put it in a 50ml measuring bottle, add pH9.

[0061] Take about 10 mg of tedizolid phosphate (TDP) and its isomer TDPEN reference substance, weigh them accurately, put them in 10 ml measuring flasks, add 2 ml of alkaline phosphatase solution, bathe in 37°C water, shake vigorously, and dissolve them at 0.5 h, 1h, 1.5h, and 2h, take 50 μl o...

Embodiment 2

[0078] Example 2 Methodological investigation of separation of tedizolid phosphate and its isomer impurities by phosphatase hydrolysis

[0079] Refer to the Chinese Pharmacopoeia 2010 edition Appendix ⅨA drug quality standard analytical method verification guidelines, to verify the determination method of tedizolid phosphate isomers, the specific content is as follows.

[0080] 1. System applicability inspection

[0081] Preparation of the mixed solution: take about 10 mg of refined tedizolid phosphate, weigh it accurately, put it in a 10 ml measuring bottle, add a precise amount of TDPEN solution (take about 10 mg of TDPEN, weigh it accurately, put it in a 10 ml measuring bottle, add buffer to dissolve and dilute to the scale, shake well, and get) 100 μl, add alkaline phosphatase solution (take appropriate amount of alkaline phosphatase, add buffer to dissolve and quantitatively dilute to make a solution with a concentration of 2 mg alkaline phosphatase per 1 ml, shake well, ...

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Abstract

The invention relates to a method of detecting tedizolid phosphate and enantiomeric impurities thereof by means of liquid chromatography. The method comprises the following steps of: 1) hydrolyzing a proper amount of tedizolid phosphate or a preparation containing tedizolid phosphate with an alkaline phosphatase solution, after reaction, adding acetonitrile to dissolve and dilute the mixture, separating an organic layer, and dissolving and diluting the mixture with absolute ethyl alcohol after drying; and 2) injecting the solution obtained in the step 1 into the liquid chromatograph to separate and determine the tedizolid phosphate and enantiomeric impurities thereof. The method provided by the invention can effectively separate and detect the content of enantiomers in a tedizolid phosphate sample, and is good in durability, so that the quality of tedizolid phosphate and preparations thereof is effectively controlled.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for measuring tedizolid phosphate and its isomer impurity content by liquid chromatography. Background technique [0002] Tedizolid phosphate (Tedizolid phosphate, formula (I)) is an oxazolidinone antibiotic developed by Cubist Pharmaceuticals, which was approved by the FDA on June 10, 2014. The trade name is Sivextro, for the treatment of acute bacterial skin and skin structure infections caused by Staphylococcus aureus and Gram-positive bacteria such as various Streptococcus species and Enterococcus faecalis. Tedizolid phosphate belongs to the oxazolidinone antibiotics, and it is not easy to produce cross-resistance with other antibiotics. Compared with the first oxazolidinone antibiotic, Linezolid, it has better efficacy and higher safety. [0003] [0004] The molecular structure of tedizolid phosphate contains a chiral carbon atom, and there is a pair of enantiomers...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 张峰骆杨丽杨谋伟朱素华薛峪泉刘春猛
Owner NANJING YOUKE BIOLOGICAL MEDICAL RES
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