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Method for simultaneously determining concentrations of ticagrelor and active metabolites and endogenous adenosine thereof in human plasma by liquid chromatography-mass spectrometry

A technology of ticagrelor and liquid chromatography-mass spectrometry, applied in the field of medical testing

Active Publication Date: 2020-06-05
SHANGHAI CHANGHAI HOSPITAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no relevant report about the method of the present invention for the simultaneous determination of ticagrelor, its active metabolites and endogenous adenosine concentrations in human plasma by liquid chromatography-mass spectrometry

Method used

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  • Method for simultaneously determining concentrations of ticagrelor and active metabolites and endogenous adenosine thereof in human plasma by liquid chromatography-mass spectrometry
  • Method for simultaneously determining concentrations of ticagrelor and active metabolites and endogenous adenosine thereof in human plasma by liquid chromatography-mass spectrometry
  • Method for simultaneously determining concentrations of ticagrelor and active metabolites and endogenous adenosine thereof in human plasma by liquid chromatography-mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 Pre-experiment

[0048] 1. Experimental materials

[0049] 30% perchloric acid, 30% acetonitrile, 50% acetonitrile, 80% acetonitrile, 100% acetonitrile, ticagrelor, AR-C124910XX

[0050] 2. Experimental method

[0051] Adenosine in the sample to be tested is unstable, so the present invention selects 30% perchloric acid to precipitate protein, effectively removes enzymes in biological samples, and ensures that the concentration of adenosine is stable after pretreatment.

[0052] 3. Experimental results

[0053] In the present invention, adenosine to be tested is a very polar compound, and ticagrelor and its active metabolites are very weak in polarity. Therefore, the present invention investigates the ratio of organic solvents in different proportions. After dissolving perchloric acid, its extraction and recovery The rate difference can be seen in Table 1.

[0054] Table 1, different proportions of acetonitrile-aqueous solution dissolved perchloric acid...

Embodiment 2

[0058] Embodiment 2 Selectivity and linearity test

[0059] 1. Experimental method

[0060] Biological blank matrix treatment: put the plasma sample for a period of time until the adenosine disappears completely (2 hours after the adenosine disappears completely), add 50μl stabilizer to 1ml of plasma, mix the plasma and set aside.

[0061] Linearity test:

[0062] Configure a series of standard curve plasma samples, including adenosine concentrations of 110, 55, 11, 5.5, 3.3, 2.2ng / mL; ticagrelor 1600, 800, 160, 80, 48, 32ng / mL; ticagrelor activity Metabolites 1108, 554, 110.8, 55.4, 33.2, 22.2 ng / mL. According to the plasma sample pretreatment operation. Taking the concentration of the analyte (C, ng / mL) as the abscissa, and the ratio (As / Ai) of the peak area of ​​the analyte (As) to the internal standard peak area (Ai) as the ordinate, use weighting (weighting factor: 1 / C 2 ) least squares method for linear regression, regression equation correlation coefficient (r) gr...

Embodiment 3

[0069] Embodiment 3 extracts recovery rate and matrix effect

[0070] 1. Experimental method

[0071] Take the blank plasma treated with the blank matrix, except that the standard series solution and the internal standard solution are not added, and the supernatant is prepared according to the "plasma sample pretreatment method" in Example 2. Add the corresponding concentration standard series solution and internal standard to the supernatant, analyze 5 samples for each concentration, and obtain the corresponding peak area value A. Take 200 μL of blank plasma treated with blank matrix, prepare standard series solutions and internal standard solutions of corresponding concentrations, operate according to the "plasma sample pretreatment method" in Example 2, analyze 5 samples for each concentration, and obtain the corresponding peak area value B. In addition to preparing standard series solutions and internal standard solutions of corresponding concentrations, analyze 5 samples...

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Abstract

The invention relates to the technical field of medical examination, and specially relates to a method for simultaneous determining concentrations of ticagrelor and active metabolites and endogenous adenosine thereof in human plasma by liquid chromatography-mass spectrometry. The concentrations of ticagrelor, active metabolites of ticagrelor and endogenous adenosine in human plasma are simultaneously determined by adopting a liquid chromatography-mass spectrometry technology. The method comprises the following steps: A, simultaneously determining the concentrations of ticagrelor, active metabolites of ticagrelor and endogenous adenosine in human plasma; B, all the samples to be detected can be subjected to peak determination under the same chromatographic and mass spectrometric conditions;and C, simultaneously extracting to-be-detected substances with different polarities in the sample. The method has the advantages that the adenosine concentration change in the blood plasma in the body of the patient and the relationship between the adenosine concentration change and the concentration of the ticagrelor and the active metabolite thereof in the blood plasma after the antiplatelet drug ticagrelor is taken can be accurately, simply, conveniently and quickly evaluated. In addition, pretreatment and chromatographic and mass spectrometric conditions are optimized, so that the determination method is simple, quick and sensitive to operate, high in specificity and good in repeatability.

Description

technical field [0001] The invention relates to the technical field of medical testing, in particular to a method for simultaneously determining the concentrations of ticagrelor, its active metabolites and endogenous adenosine in human plasma by liquid chromatography-mass spectrometry. Background technique [0002] Ticagrelor has a dual mechanism of action on platelet aggregation. On the one hand, it can block adenosine monophosphate (ADP)-induced platelet aggregation by inhibiting P2Y12 receptors. On the other hand, it can inhibit the reuptake of adenosine by ENT-1 on red blood cells. and inhibit platelet aggregation. In addition to the prototype drug itself, ticagrelor's active metabolite AR-C124910XX can also effectively inhibit platelet aggregation. These drug characteristics make it possible for ticagrelor to significantly reduce cardiovascular mortality, as well as stroke and death caused by cardiovascular events, compared with other antiplatelet drugs such as aspirin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 王卓张文静高丽红曹爱霖许小建仰先蜜毕娟杨云云丁楠邓敏
Owner SHANGHAI CHANGHAI HOSPITAL
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