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A method for the simultaneous determination of epinephrine and its metabolites based on LC-MC/MS

A technology for epinephrine and metabolites, which is applied in the field of chemical analysis and detection, can solve the problems of small application range, low absolute recovery rate, large deviation of quantitative results, etc., and achieves good application prospects, reduced matrix effects, and strong qualitative ability.

Active Publication Date: 2022-02-25
CHINA MEAT RES CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex matrix conditions of animal-derived foods, and the high polarity and small molecular weight of epinephrine, 4-hydroxy-3-methoxymandelic acid and 3,4-dihydroxymandelic acid, it is easy to cause serious problems in the analysis. matrix effect, resulting in low absolute recovery; in addition, this method uses external standard method for quantification and high-resolution mass spectrometry for analysis, so there are certain errors in the quantitative results measured by the above method, especially the quantitative results of samples near the limit of quantification The deviation will be large; in addition, this method is limited to the detection of pork samples, and the scope of application is small

Method used

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  • A method for the simultaneous determination of epinephrine and its metabolites based on LC-MC/MS
  • A method for the simultaneous determination of epinephrine and its metabolites based on LC-MC/MS
  • A method for the simultaneous determination of epinephrine and its metabolites based on LC-MC/MS

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Embodiment 1

[0065] This embodiment provides a method for the simultaneous determination of epinephrine and its metabolites based on LC-MC / MS, specifically as follows:

[0066] (1) Extraction: Weigh 2.5g sample into a 50mL centrifuge tube, add 0.25mL 1μg / mL internal standard mixed solution (containing 40-200μg / kg epinephrine-d3, 20-200μg / kg 4-hydroxy- 3-methoxymandelic acid-d3, 80-200μg / kg 3,4-dihydroxymandelic acid-d3), then add 10mL of extraction solvent, vortex with a vortex mixer for 1min, and then centrifuge the Place the tube in an ultrasonic cleaner for ultrasonic extraction for 20 minutes or place it in a vortex shaker for 10 minutes. After the extraction, place the centrifuge tube in a high-speed refrigerated centrifuge for 10 minutes (12000r / min). After the centrifugation, the supernatant Remove and place in a clean container;

[0067] (2) Purification: Take 3mL of the supernatant directly through the PRiME HLB solid-phase extraction column into a clean glass test tube, then tak...

experiment example 1

[0091] Experimental Example 1 Example 1 Precision and Recovery Experiment

[0092] This experimental example utilizes the method of embodiment 1 to measure adrenaline and metabolites thereof in pork, pork liver, milk, chicken respectively; Details are as follows:

[0093] (1) Utilize the method of embodiment 1 to detect adrenaline and metabolites thereof in pork; Each pork sample is prepared 6 parallel samples according to the spiked concentration (low, medium, high three spiked concentrations), respectively, with standard curve Calculate the concentration of the quality control spiked sample to obtain the recovery precision (RSD) of the method, and the results are shown in Table 3;

[0094] (2) Using the method of Example 1 to detect adrenaline and its metabolites in pig liver; each pig liver sample was prepared with 6 parallel samples according to the spiked concentration (low, medium, high three spiked concentrations), to The standard curve calculates the concentration of ...

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Abstract

The present invention relates to the field of chemical analysis and detection, in particular to a method for the simultaneous determination of adrenaline and its metabolites based on LC-MC / MS; the method of the present invention includes the step of preprocessing the sample, and the preprocessing includes: (1) Extraction: add the extraction solvent after adding the internal standard mixed solution in the sample, the solid-liquid ratio of the described sample and the internal standard mixed solution is 5~15g / mL, the solid-liquid ratio of the described sample and the extraction solvent is 1: 3~5g / mL; the internal standard mixed solution contains 40~200μg / kg epinephrine-d 3 , 20-200 μg / kg of 4-hydroxy-3-methoxymandelic acid-d 3 , 80~200μg / kg of 3,4-dihydroxymandelic acid-d 3 , the extraction solvent is a mixture of acetonitrile and water; (2) purification: using PRiME HLB solid-phase extraction column. The method of the invention can effectively reduce the matrix effect, and simultaneously qualitatively and quantitatively detect the epinephrine and its metabolites; the method is simple in operation, high in sensitivity, strong in qualitative ability, and accurate in quantification, and has good application prospects in the field of food safety detection.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a method for simultaneously measuring epinephrine and its metabolites based on LC-MC / MS. Background technique [0002] As a veterinary prescription drug, epinephrine hydrochloride is mainly used for emergency treatment of animal cardiac arrest, to relieve the symptoms of severe allergic diseases, and to be compatible with local anesthetics to prolong the duration of local anesthesia. It is an important veterinary prescription drug. Also an endogenous α and β receptor agonist. Due to the low oral absorption rate of epinephrine, subcutaneous injection is generally used clinically, and the effect is marked in 3 to 5 minutes, and the effect can be maintained for 1 hour. After injection, it will be rapidly inactivated by catechol-O-methyltransferase and monoamine oxidase in blood and tissues, and converted into metabolites 3,4-dihydroxymandelic acid, methoxyepinephrine ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 王守伟李石磊郭文萍李莹莹赵文涛李志刚王娟强张颖颖郭超任南陈超
Owner CHINA MEAT RES CENT
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