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High-resolution mass spectrometric detection method for fentanyl drugs in health care products

A high-resolution mass spectrometry and detection method technology, applied in the field of health care product detection, can solve the problems of inability to extract and purify fentanyl drugs, complex components, and inapplicability

Active Publication Date: 2021-09-10
西安海关技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ingredients in health care products are complex, especially those containing plant extracts. Liquid-liquid extraction alone cannot achieve the extraction and purification of fentanyl in the test substance.
Therefore, the pretreatment methods for samples such as blood, urine, and environmental water in the prior art are not suitable for the detection of fentanyl drugs in health products
In addition, the currently used triple quadrupole mass spectrometry detection technology is based on its quantitative / qualitative ion pair detection, the mass number is accurate to 1 decimal place, and there are certain defects in the determination of false positives and false negatives

Method used

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  • High-resolution mass spectrometric detection method for fentanyl drugs in health care products
  • High-resolution mass spectrometric detection method for fentanyl drugs in health care products
  • High-resolution mass spectrometric detection method for fentanyl drugs in health care products

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Embodiment 1

[0050] High-resolution mass spectrometry detection of fentanyl drugs in health products, internal standard method / MCX solid phase extraction column.

[0051] 1. Preparation of internal standard working solution

[0052] Internal standard working solution (1.0μg / mL): Measure 1mL of fentanyl-D5 internal standard stock solution, dilute it to the mark with methanol in a 10mL volumetric flask, and prepare an internal standard intermediate solution with a concentration of 10.0μg / mL , and then measure 1.0mL of the intermediate solution into a 10mL volumetric flask, and shake well to obtain a 1.0μg / mL internal standard working solution. Store in the dark at 0℃~4℃, valid for 6 months.

[0053] 2. Sample pretreatment

[0054] Liquid sample: Accurately weigh 5.00 g of liquid sample and place it in a 50 mL centrifuge tube, add 40 μL of fentanyl-D5 internal standard working solution (concentration 1.0 μg / mL), add 20 mL of acetonitrile aqueous solution (75% by volume), vortex Rotate and ...

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Abstract

The invention provides a high-resolution mass spectrometric detection method for fentanyl drugs in health-care products. The method comprises the following steps: S1, adding an internal standard into a sample to be detected, and extracting; enabling the supernate to pass through an MCX solid-phase extraction column, leaching, eluting, removing a solvent, dissolving residues, and filtering to obtain a sample solution; s2, diluting the mixed standard working solution and the internal standard working solution to prepare a series of standard working solutions of 0.01-10ng / mL; s3, detecting and analyzing the standard working solution and the sample solution; s4, performing linear regression analysis on the peak area ratio of the to-be-detected component to the internal standard substance in the standard solution and the concentration of the to-be-detected component; and S5, substituting the peak area ratio of the to-be-detected component in the sample to the internal standard substance into the standard curve linear regression equation, and calculating to obtain the concentration of the to-be-detected component. According to the method, an internal standard method is combined with an MCX cation solid-phase extraction column so that the matrix effect influence of the health care product is eliminated, and accurate quantification is realized by combining a high-resolution mass spectrum with a PRM technology.

Description

technical field [0001] The invention relates to the technical field of health care product detection, in particular to a high-resolution mass spectrometry detection method for fentanyl drugs in health care products. Background technique [0002] Fentanyl-like substances belong to a large class of opioid compounds. There are 3 varieties of fentanyl, remifentanil and sufentanil approved for marketing in my country as drugs, and alfentanil is still in the stage of drug research and development. Commonly used dosage forms in the world include injections, transdermal patches, sublingual tablets, and nasal sprays. Among them, fentanyl is often used for narcotic analgesia in advanced cancer in clinical medicine. However, fentanyl-like substances have the remarkable characteristics of opioid compounds-easy to become addicted, strong dependence, difficult to withdraw, and large doses can also lead to coma, respiratory depression, and even death. Therefore, fentanyl-like substances...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/86G01N30/34G01N30/88
CPCG01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/8634G01N30/34G01N30/8679G01N30/88G01N2030/045G01N2030/062G01N2030/146G01N2030/884
Inventor 张璐师亮何强王菡施妍婧梁靓李子豪
Owner 西安海关技术中心