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Method for measuring concentration of phenylephrine in plasma by LC-MS/MS, and pretreatment method of sample

A technology for phenylephrine and samples, which is applied in the field of medical testing, can solve the problems of inability to accurately measure the concentration of phenylephrine, incomplete separation of target compounds and impurities, and high quantitative limit of detection methods, so as to achieve rapid and effective detection and reduce detection The effect of limiting and improving specificity

Active Publication Date: 2019-01-11
CHINA RESOURCES SANJIU MEDICAL & PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For this reason, the technical problem to be solved by the present invention is that the pretreatment method of the sample adopted by the concentration detection method in the prior art does not completely separate the target compound and impurities, which leads to high quantification limit and low sensitivity of the detection method, which cannot be accurate. Determination of the concentration of low-level phenylephrine in plasma samples, thereby providing a pretreatment method for samples of phenylephrine in plasma, especially suitable for the method of LC-MS / MS determination of phenylephrine in plasma

Method used

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  • Method for measuring concentration of phenylephrine in plasma by LC-MS/MS, and pretreatment method of sample
  • Method for measuring concentration of phenylephrine in plasma by LC-MS/MS, and pretreatment method of sample
  • Method for measuring concentration of phenylephrine in plasma by LC-MS/MS, and pretreatment method of sample

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Effect test

Embodiment 1

[0067] Collection of plasma samples to be tested: 12 subjects were fasted overnight for at least 10 hours the day before the administration, and at 0 min, the subjects took renin Namin tablets (batch number: 20170401, each containing hydrochloric acid to Oxynephrine 5mg), each subject was given one tablet, and the subject’s forearm vein was embedded with an indwelling needle. 1 mL of blood was collected at different time points at 40, 60, 90, 120, 240, 360, and 480 min, and placed in a 2 Put in vacuum blood collection tubes with EDTA anticoagulant, mix well, let stand, centrifuge, take 200 μL of the upper layer of plasma, cover the tube tightly, and store in an ultra-low temperature freezer at -60°C to -90°C.

[0068] The method for measuring the concentration of phenylephrine in plasma by LC-MS / MS described in this embodiment specifically includes the following steps:

[0069] (a) Sample pretreatment

[0070] (1) Preparation of standard curve samples: Accurately weigh pheny...

Embodiment 2

[0085] Collection of plasma samples to be tested: 12 subjects were fasted overnight for at least 10 hours the day before the administration, and at 0 min, the subjects took renin Namin tablets (batch number: 20170301, each containing hydrochloric acid to Oxynephrine 10mg), each subject took one tablet, and the subjects were respectively before administration (0min) and after administration 10, 15, 20, 25, 30, 40, 60, 90, 120, 240, 1 mL of blood was collected at different time points at 360 and 480 min, and placed in a 2 Put in vacuum blood collection tubes with EDTA anticoagulant, mix well, let stand, centrifuge, take 200 μL of the upper layer of plasma, cover the tube tightly, and store in an ultra-low temperature freezer at -60°C to -90°C.

[0086] The method for measuring the concentration of phenylephrine in plasma by LC-MS / MS described in this embodiment specifically includes the following steps:

[0087] (a) Sample pretreatment

[0088] (1) Preparation of standard curv...

Embodiment 3

[0101] Collection of plasma samples to be tested: 12 subjects were fasted overnight for at least 10 hours the day before the administration, and at 0 min, the subjects took renin Namin tablets (batch number: 20170402, each containing hydrochloric acid to Oxynephrine 20mg), each subject took one tablet, and the subjects were respectively before administration (0min) and after administration 10, 15, 20, 25, 30, 40, 60, 90, 120, 240, 1 mL of blood was collected at different time points at 360 and 480 min, and placed in a 2 Put in vacuum blood collection tubes with EDTA anticoagulant, mix well, let stand, centrifuge, take 200 μL of the upper layer of plasma, cover the tube tightly, and store in an ultra-low temperature freezer at -60°C to -90°C.

[0102] The method for measuring the concentration of phenylephrine in plasma by LC-MS / MS described in this embodiment specifically includes the following steps:

[0103] (a) Sample pretreatment

[0104] (1) Preparation of standard curv...

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Abstract

The invention relates to the technical field of medical detection, and specifically relates to a method for measuring the concentration of phenylephrine in plasma by LC-MS / MS. The method comprises thefollowing steps: primary extraction: adding an internal standard working solution and an extracting solution into a sample, centrifugally layering the solution after mixing the solutions uniformly, and collecting the supernatant to obtain first supernatant; derivatization reaction: concentrating and drying the first supernatant, adding a NaHCO3 buffer salt for dissolution, and then adding an acetonitrile solution of dansyl chloride to perform a derivatization reaction; and secondary extraction: adding the extracting solution into the reaction solution after the derivatization reaction for secondary extraction, centrifuging to obtain second supernatant, concentrating and drying the second supernatant, and redissolving the product to obtain a sample solution. By adoption of the pretreatment method of the sample provided by the invention, the extraction rate of low-level phenylephrine can be maximally improved, the interference of a plasma matrix is effectively removed, the specificityis improved, the minimum detection limit is reduced to 0.02ng / ml, and the sensitivity is increased to 0.1nM to adapt to the detection requirements of the concentration of the low-concentration phenylephrine in drug clinical studies.

Description

technical field [0001] The invention belongs to the technical field of medical detection, and in particular relates to a method for measuring the concentration of phenylephrine in blood plasma by LC-MS / MS, and an applicable pretreatment method for analyzing biological samples. Background technique [0002] Phenylephrine is a catecholamine selective α1 receptor agonist, mainly used to prevent and treat hypotension caused by spinal anesthesia, general anesthesia, application of chlorpromazine, etc. It is also used for supraventricular tachycardia and mydriasis Check, phenylephrine is an over-the-counter drug that can be substituted for pseudoephedrine. [0003] Currently, the phenylephrine-like nasal decongestants used clinically usually need to be administered every four hours to relieve nasal congestion due to the short plasma half-life of the active ingredient phenylephrine in the body. Therefore, in order to delay the release time, improve the therapeutic effect and reduc...

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 陈光磊李黎王勇马鹏岗杨彦佳
Owner CHINA RESOURCES SANJIU MEDICAL & PHARMA
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