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Analysis method for reducing matrix effect of cyclosporin determination of whole blood

An analytical method and matrix effect technology, applied in the field of analysis, can solve the problems of cumbersome operation, unenvironmental protection and high cost

Active Publication Date: 2020-10-23
THE SECOND XIANGYA HOSPITAL OF CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Analysis method for reducing matrix effect of cyclosporin determination of whole blood
  • Analysis method for reducing matrix effect of cyclosporin determination of whole blood
  • Analysis method for reducing matrix effect of cyclosporin determination of whole blood

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Effect test

Embodiment 1

[0078] 1.1 Materials and methods

[0079] 1.1.1 Reference substances and reagents

[0080] CyA reference substance (Fujian Institute of Microbiology, content 98.6%, batch number 180501), CyC reference substance (Fujian Institute of Microbiology, content 94.7%, batch number 180501(S)). Rubidium acetate (analytical grade, batch number 20140226). Methanol (chromatographically pure), acetonitrile (chromatographically pure), ultrapure water (prepared by the British ELGAOQ007XXM1 pure water instrument).

[0081] 1.1.2 Instruments

[0082] Acquity UPLC TM / QuattroPremier XE micromass Technologies (LC / MS / MS) system with Masslynx V 4.1 working software (Waters, USA); low-temperature high-speed refrigerated centrifuge (Sigma, 3-18K, Germany); GH-202 electronic analytical balance (AND, Japan); VORTEX-5 vortex oscillator (Qilin Bell, Haimen City); cyano (CN) chromatographic column (100mm×2.0mm, 3.0μm, American Philome Corporation); Sanyo low-temperature refrigerator (Japan Sanyo Corpo...

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Abstract

The invention belongs to the technical field of analysis, and particularly discloses an analysis method for reducing the matrix effect of cyclosporin determination of whole blood. The analysis methodcomprises the following steps: mixing a sample to be detected with rubidium salt, ionizing to form an Rb < + >-Cy adduct from cyclosporin in the sample, and carrying out mass spectrometric analysis, wherein the rubidium salt is monocarboxylate of rubidium ions. Innovative discovery of the invention shows that under the monocarboxylate of rubidium ions, the Rb < + > and cyclosporin can be subjectedto ionization adduct accidentally and preferentially to form an Rb < + >-Cy adduct based on the special ionic characteristics and ionization characteristics, interference ions such as Na < + > and K< + > remaining in an analysis system can be competitively inhibited, cyclosporin is ionized in an expected and controllable direction, and the abundance stability of quantitative target ions is keptso that the purpose of reducing the matrix effect of a cyclosporin whole blood sample is achieved.

Description

technical field [0001] The invention belongs to the technical field of analysis and relates to a method for determining cyclosporine. Background technique [0002] Cyclosporin A (cyclosporin A, CyA) is a cyclic undecapeptide isolated from secondary metabolites of filamentous fungi, which is highly hydrophobic. Because of its excellent immunosuppressive effect, it has been used in the treatment of graft-versus-host disease since 1982, opening the CyA era of organ transplantation. In addition, CyA also has good therapeutic value for autoimmune diseases such as psoriasis, rheumatoid arthritis, and Sjogren's syndrome. Although new immunosuppressants have come out continuously, CyA is still the most prescribed immunosuppressant for organ transplantation and autoimmune diseases in the world. However, there are two relatively big problems in the clinical application of CyA. One is that its therapeutic index is narrow. If the blood drug concentration is too low, the immunosuppress...

Claims

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Application Information

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Patent Type & Authority Applications(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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