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Method for measuring epothilone B

A technology of epothilone and mobile phase, which is applied in the field of medicine and health and analysis and detection, can solve the problems of long analysis time, large amount of sample consumption, large consumption of solvent, etc., and achieve good reproducibility, high recovery rate and method operation strong effect

Inactive Publication Date: 2018-06-12
贯虹科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Epothilone is mainly obtained by microbial fermentation, and the commonly used detection method is high-performance liquid chromatography (HPLC) analysis method, but it has the disadvantages of long analysis time, large sample consumption, and large solvent consumption.

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  • Method for measuring epothilone B
  • Method for measuring epothilone B
  • Method for measuring epothilone B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Preparation of sample solution:

[0056] Preparation of the test solution: Accurately weigh 1.0 mg of Epo B sample, dissolve it in methanol, and prepare a sample solution with a concentration of 1.0 mg / mL;

[0057] (2) Preparation of reference substance solution:

[0058] Accurately weigh 2 mg of reference substances of Epo A and Epo B, dissolve them in methanol respectively, prepare a reference substance solution with a concentration of 1.0 mg / mL, draw 1 mL respectively, mix and prepare a mixed reference substance solution.

[0059] (3) Set up ultra-high performance liquid chromatography analysis conditions

[0060] Main analytical instruments: ultra-high pressure liquid chromatography system (Agilent 1290 ultra-high performance liquid chromatography), ultra-low residue autosampler, diode array detection, quadrupole-time-of-flight tandem liquid mass spectrometry (Agilent 6530Q-TOF) .

[0061] UPLC analysis conditions: Ultra-high performance liquid chromatography...

Embodiment 2

[0071] (1) Preparation of sample solution:

[0072] Preparation of the test solution: Accurately weigh 1.0 mg of Epo B sample, dissolve it in methanol, and prepare a sample solution with a concentration of 2.0 mg / mL;

[0073] (2) Preparation of reference substance solution:

[0074] Accurately weigh 2 mg of reference substances of Epo A and Epo B, dissolve them in methanol respectively, prepare a reference substance solution with a concentration of 1.0 mg / mL, draw 1 mL respectively, mix and prepare a mixed reference substance solution.

[0075] (3) Set up ultra-high performance liquid chromatography analysis conditions

[0076] Main analytical instruments: ultra-high pressure liquid chromatography system (Agilent 1290 ultra-high performance liquid chromatography), ultra-low residue autosampler, diode array detection, quadrupole-time-of-flight tandem liquid mass spectrometer (Agilent 6530 Q-TOF ).

[0077] UPLC analysis conditions: Ultra-high performance liquid chromatograph...

Embodiment 3

[0086] (1) Preparation of sample solution:

[0087] Preparation of the test solution: Accurately weigh 1.0 mg of Epo B sample, dissolve it in methanol, and prepare a sample solution with a concentration of 1.0 mg / mL;

[0088] (2) Preparation of reference substance solution:

[0089] Accurately weigh 2 mg of reference substances of Epo A and Epo B, dissolve them in methanol respectively, prepare a reference substance solution with a concentration of 1.0 mg / mL, draw 1 mL respectively, mix and prepare a mixed reference substance solution.

[0090] (3) Set up ultra-high performance liquid chromatography analysis conditions

[0091] Main analytical instruments: ultra-high pressure liquid chromatography system (Agilent 1290 ultra-high performance liquid chromatography), ultra-low residue autosampler, diode array detection, quadrupole-time-of-flight tandem liquid mass spectrometry (Agilent 6530Q-TOF) .

[0092] UPLC analysis conditions: ultra-high performance liquid chromatography...

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Abstract

The invention discloses a method for measuring epothilone B. The method comprises the following steps of: (1) preparing sample solution; (2) setting ultra-high performance liquid chromatographic analysis conditions, wherein a mobile phase A is aqueous solution of 0.1-0.5% (V / V) formic acid, and a mobile phase B is methanol or acetonitrile; adopting a bonded-phase chromatographic column; adopting amode of gradient elution; (3) setting time-of-flight tandem mass spectrometric analysis conditions, wherein an ESI ionization mode is adopted; ion monitoring is selected as a scanning mode; the massspectrum peak of the monitored ions is m / z 508.27; the operation time is 14-16 minutes; (4) measuring a group of standard epothilone B solutions with the concentrations increased in sequence, thus drawing out a standard curve of the epothilone B; (5) measuring the sample solution and calculating the content of the epothilone B from a standard curve according to detection data. The method for measuring the epothilone B disclosed by the invention has the beneficial effects that the detection can be finished in 15 minutes, the implementation is simple and easy, the method operability is strong, the recovery rate is high and the reproducibility is good.

Description

technical field [0001] The invention belongs to the technical field of medical hygiene and analysis and detection, and in particular relates to a method for measuring epothilone B. Background technique [0002] Epothilone (epothilone) is a class of macrolide compounds, first reported in 1993 by G. Höfle et al. of the German National Center for Biotechnology (GBF). Epothilone can be isolated from the fermentation broth of Somol cellulosus strain of Myxobacteria suborder, and its main components are Epothilone A (Epo A) and Epothilone B (Epo B), molecular structure: [0003] [0004] Their activity of paclitaxel-like tubulin polymerization and inhibition of microtubule depolymerization makes it a new generation of anti-mitotic drugs, and its mechanism of action is similar to that of paclitaxel drugs. This leads to apoptosis of cancer cells. Epothilone is superior to paclitaxel in terms of anti-tumor spectrum, anti-tumor activity, safety, water solubility and synthesis met...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 张春颖
Owner 贯虹科技有限公司
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