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Method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry and application

A technology of high-performance liquid chromatography and tandem mass spectrometry, which is applied in the field of detection of ketoprofen in plasma by high-performance liquid chromatography-tandem mass spectrometry, can solve the problems of high concentration of detection limit, large amount of sample required, and low sensitivity. The effect of low detection limit, fast analysis time, and broad application prospects

Inactive Publication Date: 2018-11-16
FOSHAN NANHAI EASTERN ALONG PHARMA CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The first object of the present invention is to provide a kind of method utilizing high performance liquid chromatography-tandem mass spectrometry to detect ketoprofen in blood plasma, to alleviate the detection method sensitivity that exists in the prior art is not high, the concentration of detection limit is high, detects Long time, technical problems requiring large sample volume

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  • Method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry and application
  • Method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry and application
  • Method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry and application

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preparation example Construction

[0070] In a specific embodiment, the preparation method of ketoprofen standard solution comprises:

[0071] Accurately weigh 10.0 mg of ketoprofen standard substance, place it in a 10 mL brown volumetric flask, dissolve it with an appropriate amount of methanol, and then adjust the volume to the mark to prepare a 1.0 mg / mL ketoprofen standard solution.

[0072] The ketoprofen standard solution is stored at -20°C and is valid for 3 months.

[0073] In a preferred embodiment, the ketoprofen-D3 standard substance is dissolved in low-carbon alcohol to prepare a ketoprofen-D3 alcohol solution with a concentration of 0.1-2.0 mg / mL to obtain a ketoprofen internal standard solution.

[0074] Preferably, the concentration of ketoprofen-D3 alcohol solution is 0.5-1.5 mg / mL, for example, but not limited to 0.5 mg / mL, 0.8 mg / mL, 1.0 mg / mL, 1.2 mg / mL or 1.5 mg / mL mL, preferably 0.8-1.2 mg / mL.

[0075] By optimizing the concentration of ketoprofen-D3 alcohol solution, the optimization of ...

Embodiment 1

[0117] The present embodiment provides a method for detecting ketoprofen in plasma using high performance liquid chromatography-tandem mass spectrometry, comprising the following steps:

[0118] (a), the preparation of ketoprofen standard solution:

[0119] Accurately weigh 10.0mg of ketoprofen standard substance, place it in a 10mL brown volumetric flask, dissolve it with an appropriate amount of methanol, and then adjust the volume to the mark to prepare a 1.0mg / mL ketoprofen stock solution, and store it at -20°C for later use. Valid for 3 months.

[0120] (b), the preparation of ketoprofen internal standard solution:

[0121] Accurately weigh 10.05mg of ketoprofen-D3 standard substance into a 10mL brown volumetric flask, dissolve it with an appropriate amount of methanol, and then adjust the volume to the mark to obtain a 1mg / mL ketoprofen-D3 standard solution, and store it at -20°C for later use. Valid for 3 months.

[0122] (c), pretreatment of the sample to be tested:...

Embodiment 2

[0149] In this embodiment, the specificity of the method provided by the present invention for detecting ketoprofen in plasma by using high performance liquid chromatography-tandem mass spectrometry is determined:

[0150] According to the EU Directive 2002 / 657 / EC, there should be no interfering peaks within 2.5% of the retention time deviation of the target substance in high performance liquid chromatography-tandem mass spectrometry analysis. This experiment analyzed the total ion chromatogram of the blank sample and matrix with a drug concentration of 10ng / mL, the results are as follows figure 1 , figure 2 It can be seen from the result figure that there is no interference peak in the blank sample, and the elution time of the drug added in the matrix is ​​7.04 min.

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Abstract

The invention provides a method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry and application and relates to the technical field of chemical detection. The method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry is used for taking ketoprofen-D3 as a detection internal standard and performing quantification by using an internal standard curve method. The method is high in specificity and low in detection limit; meanwhile, relevant coefficients in the linear range of a standard curve are greater than 0.999 and show that linear relation in the linear range is good and the repeatability is high; in addition, the method also has the advantages of short analysis time and low quantity of needed samples; the sample analyzing efficiency can be greatly improved; in conclusion, the whole operation process of the method for detecting ketoprofen in plasma by using high-performance liquid chromatography-tandem mass spectrometry is simple and is easy to implement; the method is scientific, reliable and controllable, is suitable for practical application and popularization and has a broad application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method and application for detecting ketoprofen in plasma by using high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Ketoprofen (Ketoprofen), also known as ketoprofen, belongs to the aryl propionic acid group and is a non-steroidal anti-inflammatory drug. White crystalline powder, odorless or almost odorless. Very soluble in methanol, easily soluble in ethanol, acetone or ether, almost insoluble in water. Ketoprofen has strong anti-inflammatory effect, few side effects and low toxicity. Its main mechanism of action is by inhibiting the cyclooxygenase pathway of arachidonic acid, which leads to the reduction of inflammatory factors, such as prostaglandins and thromboxanes. This mechanism of action results in anti-inflammatory, antipyretic and analgesic effects. [0003] At present, ketoprofen is used more and more widel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/042
Inventor 叶伟庆李成应寇贺红付良凯林孝崇
Owner FOSHAN NANHAI EASTERN ALONG PHARMA CO LTD
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