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Method for detecting isosorbide nitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in blood plasma

A technology of isosorbide dinitrate and a detection method, applied in the field of medicine, can solve the problems of low concentration, weak retention, poor signal response and the like, and achieves the effects of high sensitivity, simple operation and simple pretreatment

Active Publication Date: 2020-01-07
湖南恒兴医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, it is urgent to develop a method to solve the problems of weak retention and poor signal response of the original drug isosorbide dinitrate and two metabolites 5-isosorbide mononitrate and 2-isosorbide mononitrate; Isosorbide and 2-isosorbide mononitrate need to achieve complete liquid phase separation; the concentration of the original drug and metabolite 2-isosorbide mononitrate in the body is low, and the detection sensitivity is problematic. Accurate determination of isonitrate in plasma Concentrations of sorbide and the two metabolites 5-isosorbide mononitrate and 2-isosorbide mononitrate

Method used

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  • Method for detecting isosorbide nitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in blood plasma
  • Method for detecting isosorbide nitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in blood plasma
  • Method for detecting isosorbide nitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in blood plasma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Human K 2 Determination of the concentration of isosorbide dinitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in EDTA plasma

[0043] 1. Experimental materials and analytical equipment

[0044] Isosorbide dinitrate (analyte), 5-isosorbide mononitrate (analyte), 2-isosorbide mononitrate (analyte): China National Institute for Food and Drug Control.

[0045] Isosorbide Dinitrate- 13 C 6 (internal standard), 5-isosorbide mononitrate- 13 C 6 (internal standard), 2-isosorbide mononitrate- 13 C 6 (internal standard): Toronto Research Chemicals.

[0046] The reagents used are shown in Table 1 below:

[0047] Table 1 Reagents

[0048]

[0049] Note: Reagents of the same grade or higher can also be used

[0050] The equipment used is shown in Table 2 below:

[0051] Table 2 Instruments and equipment

[0052]

[0053]

[0054] Note: Equipment of the same level or higher can also be used.

[0055] 2. Liquid conditions

[0056] 2.1. S...

Embodiment 2

[0175] Take the 300 μL quality control sample (QCM) obtained in Table 7 by the method of Example 1, add 10 uL of 500 / 500 / 500ng / uL internal standard isosorbide dinitrate- 13 C 6 / 5-isosorbide mononitrate- 13 C 6 / 2-isosorbide mononitrate- 13 C 6 Working solution, vortex and mix well, add 1250uL ethyl acetate to the sample, vortex for 15min, centrifuge at 15700g for 10min; take 900uL of the supernatant to a 96 deep-well plate, blow dry with nitrogen; add 100μL of 10% acetonitrile -Water redissolution, vortex 10min; Take 20uL sample to analyze and detect isosorbide dinitrate, 2-isosorbide mononitrate, 5-isosorbide mononitrate, it can be known that the chromatographic columns with different column lengths have a greater impact on the method Big.

[0176] When using a chromatographic column with a column length of 75mm, such as Figure 5-1 , Figure 5-2 , Figure 5-3 As shown, the chromatographic peaks and interference peaks of 2-isosorbide mononitrate and 5-isosorbide mono...

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Abstract

The invention provides a method for detecting and analyzing isosorbide dinitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate in blood plasma. According to the method, one-step organic solution extraction is adopted, a proper chromatographic column length is selected, acetate adduct ions are used as parent ions to establish a detection channel, parameter combination is optimized, and finally, the LC-MS / MS method capable of simultaneously determining isosorbide nitrate, 2-isosorbide mononitrate and 5-isosorbide mononitrate is successfully formed. The detection and analysis method hasthe advantages of being rapid, accurate, high in sensitivity, easy and convenient to operate and the like, and the blood concentration of isosorbide dinitrate, 5-isosorbide mononitrate and 2-isosorbide mononitrate can be measured at the same time.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to the LC-MS / MS analysis of isosorbide dinitrate (XSYSLZ), 5-isosorbide mononitrate (5-DXSYSLZ) and 2-isosorbide mononitrate (2-DXSYSLZ) in human plasma. MS detection method. Background technique [0002] Isosorbide dinitrate is a vasodilator whose main pharmacological action is to relax vascular smooth muscle. The overall effect is to reduce myocardial oxygen consumption, increase oxygen supply, and relieve angina. Clinically, it can be used to treat various types of coronary heart disease angina pectoris and prevent attacks. Intravenous infusion can be used in the treatment of congestive heart failure, various types of hypertensive emergencies and the control of hypertension before surgery. [0003] The main pharmacological effect of isosorbide dinitrate (ISDN) is to relax vascular smooth muscle. ISDN is metabolized in vivo to produce isosorbide mononitrate (ISMN), which rele...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54
CPCG01N30/02G01N30/06G01N30/72G01N30/54G01N2030/027G01N2030/062
Inventor 郭建军李良李长春陈梅汪牧西
Owner 湖南恒兴医药科技有限公司
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