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A method for detecting plasma concentration of nmda receptor antagonist jcc-02 based on hplc-ms/ms technology

A technology of JCC-02 and receptor antagonists, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of undiscovered pharmacokinetic characteristics, etc., and achieve short measurement time, fast and accurate methods, and simple pretreatment Effect

Active Publication Date: 2021-04-23
THE FIRST HOSPITAL OF CHINA MEDICIAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A method for detecting plasma concentration of nmda receptor antagonist jcc-02 based on hplc-ms/ms technology
  • A method for detecting plasma concentration of nmda receptor antagonist jcc-02 based on hplc-ms/ms technology
  • A method for detecting plasma concentration of nmda receptor antagonist jcc-02 based on hplc-ms/ms technology

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 present invention provides a kind of method based on HPLC-MS / MS technology detection NMDA receptor antagonist JCC-02 blood concentration, relates to the field of drug analysis, comprising the following steps: SD rats after JCC-02 intragastric administration In the blood plasma, add methanol, acetonitrile and internal standard working solution in sequence, vortex to take the supernatant and dissolve it with the mobile phase and then inject the sample. The internal standard working solution is the methanol solution of gliclazide; ‑The mixed solution of formic acid and water is used as the mobile phase for gradient elution, the Venusil ASB C8 chromatographic column is used for chromatographic separation, and the secondary mass spectrometer is used for detection and quantitative analysis. The method has strong specificity, high sensitivity, less sample volume, simple and rapid pretreatment, and short analysis cycle. The method is verified by methodology to be accurate and reliable, and is suitable for the determination of drug concentration and drug concentration of JCC‑02 in SD rat plasma. Kinetic studies.

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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Patent Type & Authority Patents(China)
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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