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HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrum/Mass Spectrum) technique-based method for detecting blood concentration of NMDA (N Methyl D Aspartate) receptor antagonist JCC-02

A JCC-02, receptor antagonist technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problem of undiscovered pharmacokinetic characteristics, and achieve the effects of short measurement time, time saving, and prevention of matrix effects

Active Publication Date: 2018-11-30
THE FIRST HOSPITAL OF CHINA MEDICIAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no domestic and foreign literature reports on the quantitative analysis method of drug concentration and preclinical pharmacokinetic characteristics in JCC-02 biological samples

Method used

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  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrum/Mass Spectrum) technique-based method for detecting blood concentration of NMDA (N Methyl D Aspartate) receptor antagonist JCC-02
  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrum/Mass Spectrum) technique-based method for detecting blood concentration of NMDA (N Methyl D Aspartate) receptor antagonist JCC-02
  • HPLC-MS/MS (High Performance Liquid Chromatography-Mass Spectrum/Mass Spectrum) technique-based method for detecting blood concentration of NMDA (N Methyl D Aspartate) receptor antagonist JCC-02

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1 methodological research

[0046] 1. Instruments and equipment:

[0047] Agilent 1290 Infinity high performance liquid chromatograph, American Agilent company;

[0048] AB API4000 triple quadrupole tandem mass spectrometer, AB Sciex, USA;

[0049] D3024R centrifuge, Beijing Dalong;

[0050] XW-80A vortex mixer, Shanghai Qingpu Huxi Instrument Factory;

[0051] CPA 124S electronic analytical balance, Germany Sartorius company;

[0052] Weight scale, Cixi Tiandong Weighing Apparatus Factory;

[0053] 2. Reagents and reagents:

[0054] JCC-02 (≥purity 98.0%), provided by the Department of Medicinal Chemistry, Shenyang Pharmaceutical University;

[0055] Gliclazide (purity 99.9%), China National Institute for the Control of Pharmaceutical and Biological Products;

[0056] Methanol (chromatographically pure), Dima Technology Co., Ltd.;

[0057] Acetonitrile (chromatographically pure), Thermo Fisher Scientific Co., Ltd.;

[0058] Formic acid (chromatograp...

example 2

[0090] Example 2 Pharmacokinetic Research

[0091] 1. Dosing regimen and sample collection

[0092] Accurately weigh 3.5 mg of JCC-02 sample, add 50 μL DMSO to dissolve, then add 500 μL Tween-80, and mix well by ultrasonic. Continue to add 2.5mL PEG-400, and ultrasonically mix again. Dilute to 50mL with pure water, mix by ultrasonic to prepare 0.07mg·mL -1 JCC-02 clarification solution.

[0093] Before the experiment, SD rats were fasted for 12 hours and had free access to water. Weigh and label 8 SD rats (4 females and 4 males) weighing 200±20g, according to 0.7mg·kg -1 The dosage is administered by intragastric administration. At the designated blood collection time points (0, 0.17, 0.33, 0.5, 0.75, 1, 1.5, 2.5, 4.5, 6.5, 9, 12 and 24 hours), blood was collected from the orbital venous plexus, and the blood volume was 0.4 mL. 1.5mL heparinized centrifuge tube. at 10000r·min -1 Centrifuge at a high speed for 10 minutes, transfer the upper layer of plasma to an empty c...

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Abstract

The invention provides an HPLC-MS / MS (High Performance Liquid Chromatography-Mass Spectrum / Mass Spectrum) technique-based method for detecting blood concentration of a NMDA (N Methyl D Aspartate) receptor antagonist JCC-02 and relates to the field of drug analysis. The method comprises the following steps of: sequentially adding methanol, acetonitrile and an internal standard working solution intoplasma of an SD (Sprague Dawley) rat after intragastric administration of the JCC-02, eddying and dissolving supernatant by using a mobile phase to obtain a preprocessed sample, wherein the internalstandard working solution was a gliclazide methanol solution; and carrying out gradient elution by taking acetonitrile-formic acid water mixed solution as a mobile phase and by adopting HPLC-MS / MS technique, carrying out chromatographic separation by using a Venusil ASB C8 chromatographic column, detecting through a second-stage mass spectrometry and carrying out quantitative analysis. The methodhas the advantages of being strong in specificity, high in sensitivity, small in sample sampling amount, simple and rapid in preprocessing and short in analysis period; and proved by methodology, themethod is accurate and reliable and is suitable for drug concentration determination of the JCC-02 in the plasma of the SD rat and pharmacokinetic study.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting blood drug concentration of NMDA receptor antagonist JCC-02 based on HPLC-MS / MS technology. Background technique [0002] Alzheimer's disease (AD) is an irreversible progressive neurodegeneration clinically manifested by progressive memory impairment, aphasia, apraxia, agnosia, impairment of visuospatial skills, executive dysfunction, and personality and behavior In recent years, its incidence has been increasing year by year. At present, only memantine, an N-methyl-D-aspartate (NMDA) receptor antagonist, is on the market for the treatment of moderate and severe AD, which is far from enough for complex clinical needs Therefore, in recent years, the research and development of NMDA receptor antagonist therapeutic drugs has become a focus of attention. [0003] According to the chemical structure of memantine, a novel NMDA receptor antagonist candidate compound...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 林建阳杨恬时月林城江阎成炟
Owner THE FIRST HOSPITAL OF CHINA MEDICIAL UNIV
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