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An Analytical Method for Subtracting the Matrix Effect in Determination of Cyclosporin in Whole Blood

An analytical method and technology of matrix effect, applied in the field of analysis, can solve the problems of inaccurate reduction effect, high cost, large consumption of organic solvents, etc., to reduce the analysis operation process and workload, reduce the absolute matrix effect of whole blood, and pre-treatment The effect of process simplification

Active Publication Date: 2022-06-03
THE SECOND XIANGYA HOSPITAL OF CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the existing problems of large matrix effect and complex measurement process in the determination of cyclosporine in whole blood, the purpose of the present invention is to provide a method for analyzing cyclosporine in whole blood that can effectively reduce the matrix effect
[0011] The determination of cyclosporine in biological samples such as human whole blood is accompanied by severe matrix effects. The current methods for reducing the matrix effect are not specific, the reduction effect is not accurate, or additional equipment is required, the operation is cumbersome, and the efficiency is low. Low, or need to consume a lot of organic solvents to purify samples, high cost, not environmentally friendly and other major defects

Method used

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  • An Analytical Method for Subtracting the Matrix Effect in Determination of Cyclosporin in Whole Blood
  • An Analytical Method for Subtracting the Matrix Effect in Determination of Cyclosporin in Whole Blood
  • An Analytical Method for Subtracting the Matrix Effect in Determination of Cyclosporin in Whole Blood

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Experimental program
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Effect test

Embodiment 1

[0081] 1.1.2 Instruments

[0087] The column temperature of the chromatographic column: 40°C. Mobile phase: acetonitrile: rubidium acetate aqueous solution = 45:55 (V / V), flow rate: 0.4 ml·min

[0091] The mass spectrometry data acquisition mode is MRM, the Scan Time is 0.10s, and the Interscan Time is 0.005s. Span

[0093]

[0102] MF=(Set2-Set1)÷S1×100%

[0104] RE=Set3÷Set2×100%

[0105] PE=Set3÷Set1×100%

[0106] According to industry consensus and relevant rules, when absolute MF≤±15%, it can be considered that there is no significant matrix effect. no

[0112] The matrix effect data of 10 different individual source whole blood sample extracts to CyA and CyC are shown in Table 1. Low,

[0114]

[0116] The average extraction recovery rate of CyA is between 76.0% and 81.6%, and the average extraction recovery rate of CyC is between 82.3% and 82.3%.

[0117] The average treatment efficiency of CyA is between 78.9% and 81.2%, and the average treatment efficiency of CyC is be...

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Abstract

The invention belongs to the technical field of analysis, and specifically discloses an analysis method for reducing the matrix effect in the determination of whole blood cyclosporine. The sample to be tested is mixed with a rubidium salt and then ionized, so that the cyclosporine in the sample forms Rb + ‑Cy adduct, followed by mass spectrometry analysis; the rubidium salt is a monocarboxylate salt of rubidium ions. The present invention innovatively finds that under the monocarboxylate salt of rubidium ions, based on its special ion characteristics and ionization characteristics, the Rb + Unexpected preferential ionization adducts with cyclosporine to form Rb + ‑Cy adducts that can competitively inhibit residual Na in the assay system + 、K + and other interfering ions, so that cyclosporine proceeds in the expected and controllable direction during the ionization phase, and maintains the stability of the quantitative target ion abundance, thereby achieving the purpose of reducing the matrix effect of cyclosporine whole blood samples.

Description

An analytical method for reducing the matrix effect of the determination of whole blood cyclosporine technical field The invention belongs to the analytical technology field, the assay method of technical design cyclosporine. Background technique Cyclosporin A (cyclosporin A, CyA) is a cyclosporin isolated from secondary metabolites of filamentous fungi. The undecapeptide is highly hydrophobic. Because of its excellent immunosuppressive effect, it has been used in graft-versus-host since 1982. The treatment of the disease has opened the CyA era of organ transplantation. In addition, CyA is effective in psoriasis, rheumatoid arthritis, Sjögren's syndrome, etc. Autoimmune diseases also have good therapeutic value. Despite the continuous introduction of new immunosuppressants, CyA is still It is the most prescribed immunosuppressant for organ transplantation and autoimmune diseases in the world. However, there are comparisons in the clinical application of CyA The...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86G01N27/62
CPCG01N30/02G01N30/06G01N30/7266G01N30/8675G01N27/62G01N2030/045
Inventor 朱荣华李焕德方平飞张毕奎滕婧颜苗蔡骅琳彭文兴方春华
Owner THE SECOND XIANGYA HOSPITAL OF CENT SOUTH UNIV
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