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Method for separation and determination of linezolid raw material x3 and its process impurity x2

A technology of linezolid and process impurities, which is applied in the field of analytical chemistry to achieve the effects of high accuracy, effective control of impurities and shortening of separation time

Active Publication Date: 2020-09-11
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently there is no method for rapid separation of linezolid raw material (X3) and related impurities

Method used

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  • Method for separation and determination of linezolid raw material x3 and its process impurity x2
  • Method for separation and determination of linezolid raw material x3 and its process impurity x2
  • Method for separation and determination of linezolid raw material x3 and its process impurity x2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The chromatogram of embodiment 1 (S)-1-acetamido-2-acetoxy-3-chloropropane (X3) and process impurity (X2)

[0044] Mobile phase: 20% by volume acetonitrile in water.

[0045] Impurity X2 stock solution: Take 240.44mg of impurity X, weigh it accurately, put it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0046] Preparation of mixed solution: Take 20.27mg of the test product X31, weigh it accurately, put it in a 20ml measuring bottle, add 0.3ml of impurity X2 stock solution, add diluent to dissolve and dilute to the mark, and shake well.

[0047] The diluent and the mixed solution were respectively injected according to the above-mentioned chromatographic conditions, and the chromatogram was recorded. The measurement results are shown in Table 1. see results figure 1 .

[0048] Table 1 test results

[0049]

[0050] Conclusion: the blank diluent does not interfere with the determination of the sample; the...

Embodiment 2

[0051] The chromatogram of embodiment 2 (S)-1-acetamido-2-acetoxy-3-chloropropane (X3) and process impurity (X2)

[0052] Trifluoroacetic acid aqueous solution: take 0.2ml of trifluoroacetic acid and add it to 1000ml of water;

[0053] Trifluoroacetic acid acetonitrile solution: take 0.2ml trifluoroacetic acid and add it to 1000ml acetonitrile;

[0054] Mobile phase: The volume ratio of trifluoroacetic acid aqueous solution to trifluoroacetic acid acetonitrile solution is 80:20.

[0055] Impurity X2 stock solution: take 240.05 mg of impurity X, weigh it accurately, put it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0056] Preparation of mixed solution: Take 20.16 mg of the test product X3, weigh it accurately, put it in a 20ml measuring bottle, add 0.3ml of impurity X2 stock solution, add diluent to dissolve and dilute to the mark, and shake well.

[0057] The diluent and the mixed solution were respectively injec...

Embodiment 3

[0061] Embodiment 3 different mobile relative to the separation situation of X3 and impurity X2

[0062] Trifluoroacetic acid aqueous solution: take 0.2ml of trifluoroacetic acid and add it to 1000ml of water;

[0063] Trifluoroacetic acid in acetonitrile solution: Take 0.2ml of trifluoroacetic acid and add it to 1000ml of acetonitrile.

[0064] Carry out the preparation of mobile phase ratio A, B, C as shown in Table 3.

[0065] Table 3 The ratio of mobile phase

[0066] Aqueous solution of trifluoroacetic acid (V) Trifluoroacetic acid acetonitrile solution (V) A 90 10 B 80 20 C 70 30

[0067] Impurity X2 stock solution: take about 40mg of impurity X2, accurately weigh it, put it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0068] Preparation of the mixed solution: Take about 120mg of the test product X3, accurately weigh it, put it in a 20ml measuring bottle, add 0.3ml of impu...

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Abstract

The invention belongs to the field of analytical chemistry and relates to a method for separating and determining a linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3 and its process impurities X2, in particular to a method for separating and determining a linezolid raw material X3 and its process impurities X2 by adopting a high performance liquid chromatography. A chromatographic column adopted in the method uses octadecyl silane bonded silica gel as a filler, water added with an ion-pairing agent and acetonitrile which are in certain proportion are adopted as mobile phases. The method can completely separate the linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3 and the its process impurities X2, is simple, convenient, feasible, good in reproducibility and strong in specificity and can effectively determine the related substance content in the linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3.

Description

[0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring linezolid raw material (S)-1-acetylamino-2-acetoxy-3-chloropropane (X3) and its process impurity (X2). Background technique [0002] Linezolid is an oxazolidinone antibiotic drug developed by Pfizer, which was approved by the FDA in 2000 for the treatment of infections caused by Gram-positive (G+) cocci, including suspected or confirmed nosocomial infections caused by MRSA. Pneumonia (HAP), community-acquired pneumonia (CAP), complicated skin or skin and soft tissue infection (SSTI), and vancomycin-resistant enterococcus (VRE) infection, the trade name is Zyvox. For the most representative methods of preparing linezolid disclosed so far, refer to patent WO9507271 applied by Upjohn Company, patent WO9924393 and patent WO2005099353 of Pharmacia Upjohn US Company. The Chinese patent application number 201310168412.1 reports a preparation method of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/18C07C231/24G01N30/02
Inventor 林晓兵张波
Owner CHONGQING HUABANGSHENGKAI PHARM
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