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High-performance liquid chromatography-triple quadrupole mass spectrometry combination method for determining paclitaxel or paclitaxel

A technology of high-performance liquid chromatography and triple quadrupole, which is applied in the field of pharmaceutical analysis and can solve problems such as mass spectrometer contamination

Active Publication Date: 2016-03-23
FUDAN UNIV SHANGHAI CANCER CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, non-volatile reagents may contaminate the mass spectrometer

Method used

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  • High-performance liquid chromatography-triple quadrupole mass spectrometry combination method for determining paclitaxel or paclitaxel
  • High-performance liquid chromatography-triple quadrupole mass spectrometry combination method for determining paclitaxel or paclitaxel
  • High-performance liquid chromatography-triple quadrupole mass spectrometry combination method for determining paclitaxel or paclitaxel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Example 1 Mass Spectrometry Ionization Forms of Docetaxel and Paclitaxel in Different Ionization Modes

[0083] experimental method:

[0084] 1. Concentration of paclitaxel or docetaxel reference substance solution: 50 μg / mL, mixed with the liquid phase mobile phase through the T-shaped tee by needle pump injection, and then enters the mass spectrometer detector.

[0085] 2. Liquid mobile phase: solvent A: aqueous solution; solvent B: acetonitrile. The electrolytes and concentrations in solvent A are: (1) 1‰ formic acid; (2) 1‰ acetic acid; (3) 10mM ammonium formate; (4) 10mM ammonium acetate.

[0086] 3. Liquid-mass spectrometry analysis conditions: Chromatographic column: Agilent EclipseplusC 18 Column (2.1×50mm, 5μm); column temperature: 40°C; elution conditions: isocratic elution with 46.5% solvent B; flow rate: 0.40mL / min; mass spectrometry detection using ESI (+) or ESI (-) ionization mode .

[0087] 4. Needle pump speed: 10μL / min.

[0088] 5. Result represen...

Embodiment 2

[0093] Under embodiment 2ESI (-) ionization mode, the optimization of ammonium formate concentration in the liquid phase mobile phase

[0094] experimental method:

[0095] 1. Liquid-mass spectrometry analysis conditions: Chromatographic column: Agilent EclipseplusC 18 Column (2.1×50mm, 5μm); column temperature: 40°C. Liquid mobile phase: Solvent A: H 2 O or aqueous ammonium formate; solvent B: acetonitrile. Elution conditions: isocratic elution with 46.5% solvent B. Flow rate: 0.40mL / min. Injection volume: 10 μL. The mass spectrometry adopts ESI(-) ionization mode. Under the collision energy of -51V in the MRM detection mode, the m / z852→206 ion pair of docetaxel is detected; under the collision energy of -24V, the m / z898→ of paclitaxel is detected. 525 ion pairs, mass spectrometry parameters are shown in Table 3, docetaxel and paclitaxel in ESI(-) figure 2 .

[0096] Table 3: Mass Spectrometry Working Parameters for Quantitative Analysis of Docetaxel and Paclitaxel i...

Embodiment 3

[0102] Under embodiment 3APCI (-) ionization mode, the optimization of ammonium formate concentration in the liquid phase mobile phase

[0103] experimental method:

[0104] 1. Liquid-mass spectrometry analysis conditions: Chromatographic column: Agilent EclipseplusC 18 Column (2.1×50mmID, 5μm); column temperature: 45°C; mobile phase: solvent A: H 2 O or aqueous ammonium formate; solvent B: methanol. Gradient elution conditions: elution with 20% solvent B in 0~0.1min, increasing solvent B from 20% to 60% at a constant speed in 0.1~0.5min, increasing solvent B from 60% to 90% at a constant speed in 0.51~0.8min, 0.81~1.5 Min was eluted with 90% solvent B, 1.51-1.6 min, solvent B decreased from 90% to 20% at a constant speed, and 1.61-3.5 min was 20% solvent B for column equilibration; flow rate: 0.80mL / min; injection volume: 10μL. Mass spectrometry uses APCI(-) ion source, under the collision energy of -35V in the MRM detection mode, the m / z853→280 ion pair of docetaxel is de...

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Abstract

The invention relates to a method for determining paclitaxel or paclitaxel, in particular to a method for quantitatively analyzing paclitaxel or paclitaxel by adopting a high-performance liquid chromatography-triple quadrupole mass spectrometry combination technology. The method comprises the steps of using a mobile phase containing ammonium formate and formic acid in a high-performance liquid chromatograph, adopting an MRM mode to determine formate added quasi-molecular ion peaks and daughter ion peaks of the paclitaxel or paclitaxel in an ESI (-) or APCI (-) ionization mode.

Description

technical field [0001] The invention belongs to the field of drug analysis and relates to a method for determining docetaxel or paclitaxel. More specifically, it relates to a method for quantitative analysis of docetaxel or paclitaxel based on high performance liquid chromatography-triple quadrupole mass spectrometry (LC-MS) technology. Background technique [0002] Docetaxel and paclitaxel are taxane anticancer drugs, which are a class of natural products extracted from the bark of Yew brevifolia. They are clinically used to treat breast cancer, non-small cell lung cancer, pancreatic cancer, gastric cancer, ovarian cancer and head and neck cancer. cancer etc. [1-2] . Its mechanism of action is to promote tubulin to form stable microtubules by binding to tubulin of tumor cells, while inhibiting its depolymerization, blocking cell mitosis, and inhibiting and killing tumor cells [3] . [0003] According to the results of literature review, the quantitative analysis method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 孙艳王漪璇毋丹钱隽欧阳年
Owner FUDAN UNIV SHANGHAI CANCER CENT
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